Month: May 2021

Related Products of 10250-64-3,Some common heterocyclic compound, 10250-64-3, name is 1-Methyl-3-phenyl-1H-pyrazole-5-carboxylic acid, molecular formula is C11H10N2O2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

General procedure: To a solution of 19 (1.2 eq) and HOBt(1.4 eq) in DMF (0.5 M) were added EDCI (1.3 eq) and a solution of 15a-j or 16a-j (1.0 eq) in DMF (0.25 M), Et3N (3.5 eq) at 0 C. The reaction mixture was stirred at room temperature for 24 hours, then diluted in AcOEt. The organic phase was washed with water twice, saturated aqueous NaHCO3 three times, and brine, then dried over Na2SO4,filtered, and concentrated. The residue was purified by flash column chromatography to give intermediates 17a-j and 18a-j.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Methyl-3-phenyl-1H-pyrazole-5-carboxylic acid, its application will become more common.

Reference of 141573-95-7, A common heterocyclic compound, 141573-95-7, name is Ethyl 3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylate, molecular formula is C8H10F2N2O2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

l,2,3,4-tetrahydro-9-isopropyl-l,4-methanonaphthalen-5-amine320 mg (1 eq. ; 9: 1 syn:anti mixture) in 2 ml THF and 325 mg (1.6 mmol)DFMMP (1) in 2 ml THF were added to a suspension of 268mg (1.5 eq.) KOtBu in 10 ml THF at 0C. After stirring at room temperature over night the reaction mixture was poured out in water and extracted twice with acetic ether. The purified organic extracts were washed with water and a saturated NaCl solution, dried, filtered and concentrated over sodium sulphate. The residue was filtrated through a silicagel column (Si02 ; hexane/acetic ether 1 : 1) and the desired product Isopyrazam was obtained in 77 % yield (440 mg) (purity GC 100 % ; HPLC – 254nm > 99 % as 86.5: 12.7 symanti mixture).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Application of 345637-71-0, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 345637-71-0 name is 2-(5-Methyl-3-(trifluoromethyl)-1H-pyrazol-1-yl)acetic acid, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Step F: Preparation of 1-[4-[4-(4,5-dihydro-5-phenyl-3-isoxazolyl)-2-thiazolyl]-1-piperazinyl]-2-[5-methyl-3-(trifluoromethyl)-1H-pyrazol-1-yl]ethanone To a solution of 1-[4-(4,5-dihydro-5-phenyl-3-isoxazolyl)-2-thiazolyl]piperazine hydrochloride (i.e. the product of Example 7, Step E) (200 mg, 0.57 mmol) and 5-methyl-3-(trifluoromethyl)-1H-pyrazole-1-acetic acid (0.120 g, 0.57 mmol) in dichloromethane (10 mL) at room temperature was added 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride (0.110 g, 0.57 mmol), triethylamine (0.086 g, 0.85 mmol) and 1-hydroxy-benzotriazole hydrate (0.020 g, 0.14 mmol). The reaction mixture was stirred at room temperature for 24 h. The reaction mixture was diluted with dichloromethane (30 mL) and washed with water (20 mL) and brine (20 mL). The organic layer was dried (Na2SO4) and concentrated under reduced pressure. The crude residue was purified by column chromatography using 3% methanol in chloroform as eluant to give 180 mg of the title product as a white solid. 1H NMR (CDCl3): delta 2.32 (s, 3H), 3.29 (m, 1H), 3.52 (m, 2H), 3.61 (m, 2H), 3.79-3.72 (m, 5H), 4.98 (m, 2H), 5.69 (m,1H), 6.33 (s, 1H), 6.93 (s, 1H), 7.38-7.28 (m, 5H). Mass spectrum at 505.5 (M+1).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 2-(5-Methyl-3-(trifluoromethyl)-1H-pyrazol-1-yl)acetic acid, and friends who are interested can also refer to it.

Related Products of 1780-72-9, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 1780-72-9 as follows.

To a solution of 22 (14.0 g, 79.54 mmol) in ethanol (280 mL) were added ethyl acetoacetate (15.15 mL, 15.59 g, 119.79 mmol) and acetic acid (4.55 mL, 79.54 mmol) at room temperature under nitrogen atmosphere. The reaction mixture was then heated to 85 C. and stirred for 16 h. The progress of the reaction was monitored by TLC. After 16 h, the reaction mixture was concentrated completely under reduced pressure. The resultant solid was treated with CH2Cl2 (30 mL) and the solid was filtered. The filtered solid was dried under high vacuum at 45-55 C. to afford 23 (10.7 g, 55.57%) as a pale yellow solid.

According to the analysis of related databases, 1780-72-9, the application of this compound in the production field has become more and more popular.

Reference of 23170-45-8,Some common heterocyclic compound, 23170-45-8, name is Methyl 3-methyl-1H-pyrazole-4-carboxylate, molecular formula is C6H8N2O2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

N2 protection,3-methyl-1H-pyrazole-4-carboxylate(0.14 g, 1.0 mmol), CuI (19.1 mg,0.1 mmol), K2CO3 (0.29 g, 2.1 mmol)III3 (0.34 g, 1.2 mmol),(E) -N, N’-dimethyl-1,2-cyclohexyl diamine (28.5 mg, 0.2 mmol) and DMF (3 mL) were added to a 25 mL two-necked flask and reacted at 110 C for 24 h,Cooled to room temperature, diluted with 10 mL of water, extracted with ethyl acetate (15 mL x 3)Saturated brine (10 mL), dried over anhydrous magnesium sulfate, the solvent was removed by distillation under reduced pressure,Silica gel column (V ethyl acetate: V petroleum ether = 6: 1),To a solution of 0.2 g of methyl orange 1- (3′-nitro-4′-piperidine-phenyl) -3-methyl-pyrazole-4-carboxylate (IV3).

The synthetic route of 23170-45-8 has been constantly updated, and we look forward to future research findings.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 35691-93-1, name is Ethyl 3,5-dimethyl-1H-pyrazole-4-carboxylate, A new synthetic method of this compound is introduced below., Quality Control of Ethyl 3,5-dimethyl-1H-pyrazole-4-carboxylate

A mixture of 2-[2-(3-chloro-5-fluorobenzyl)-1-benzothiophen-7-yl]-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (1.50 g, 3.72 mmol), ethyl 3,5-dimethyl-1H-pyrazole-4-carboxylate (0.76 g, 4.5 mmol) and copper(II) acetate monohydrate (0.37 g, 1.9 mmol) in pyridine (8 mL) was reacted for 20 hr at 50C. The reaction solution was concentrated, and the residue was diluted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate-hexane 1:10) to give ethyl 1-[2-(3-chloro-5-fluorobenzyl)-1-benzothiophen-7-yl]-3,5-dimethyl-1H-pyrazole-4-carboxylate (0.88 g). To a solution of the compound in methanol (20 mL) was added 1N aqueous sodium hydroxide solution (12 mL, 12 mmol) at room temperature, and the mixture was stirred for 1 days at 60C. To the reaction mixture were added water and hydrochloric acid, and the aqueous layer was acidified. The mixture was extracted with ethyl acetate. The organic layer was dried over magnesium sulfate, and evaporated under reduced pressure. The obtained residue was crystallized from ether to give the title compound (630 mg, yield 41%). melting point 187 – 188C. 1H-NMR (DMSO-d6)delta: 2.38 (6 H, s), 4.29 (2 H, s), 7.18 – 7.25 (1 H, m), 7.30 (1 H, s), 7.36 – 7.44 (2 H, m), 7.46 – 7.54 (1 H, m), 7.72 – 7.81 (1 H, m), 7.88 – 7.92 (1 H, m), 12.43 (1 H, br s).

The synthetic route of 35691-93-1 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 1280210-79-8, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 1280210-79-8, name is tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-carboxylate, This compound has unique chemical properties. The synthetic route is as follows.

Dissolve 2,6-dihydropyrrolo [3,4-c] pyrazole-5(4H)-tert-butyl carboxylate (12 g, 56.7 mmol) in acetonitrile (100 mL),Add 1-bromo-3- (bromomethyl) -5-methoxybenzene 4b (19 g, 68.1 mmol), Cesium carbonate (64.8 g, 199 mmol), Nitrogen was replaced 3 times, and the reaction was performed in an 80 C oil bath for 3 hours. Filtering the reaction solution,The filtrate was concentrated. The residue was purified by column chromatography (petroleum ether: ethyl acetate = 2: 1) to obtain 2-(3-bromo-5-methoxybenzyl)-2,6-dihydropyrrolo[3,4-c]pyrazole-5(4H)-tert-butyl carboxylate 4c (23 g, yellow oil), yield: 82.9%.

The chemical industry reduces the impact on the environment during synthesis tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-carboxylate. I believe this compound will play a more active role in future production and life.

Synthetic Route of 2075-45-8, These common heterocyclic compound, 2075-45-8, name is 4-Bromo-1H-pyrazole, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

1-{[2-(trimethylsilyl)ethoxy]methyl}-1H pyrazole-4-carbaldehyde was prepared as follows: To a solution of 4-bromo pyrazole (16.90 g, 115 mmol) in THF (400 mL) under N2 at 0 C was added NaH ( 3.31 g, 138 mmol) and stirred for 15 min. Neat SEM-Cl (21.10 g, 126.46 mmol) was added drop wise to the reaction mixture and stirred overnight at rt. The reaction was quenched with water (200 mL) and excess THF was removed in vacuo. The residue was extracted with EtOAc (2×500 mL), dried over MgS04 and removed in vacuo to give crude 4- bromo- 1 – ( [2-(trimethylsilyl)ethoxy]methyl) – lH-pyrazole (36 g) as a yellow oil. The crude material was used in next step without further purification. To a solution of 4-bromo-l-{[2-(trimethylsilyl)ethoxy]methyl}-IH-pyrazole (35.83 g, 129.35 mmol) in THF (750 mL) at at -78 C under N2 was added n-BuLi (67.26 mL, 168.16 mmol, 2.5 M) slowly. After the reaction mixture was stirred for 3 h at -78 C, DMF (50 mL) was added at -78 C and warmed to rt overnight. It was cooled to -30 C, quenched with 1 N HCl (120 mL) and stirred at 0 C for 30 min and 30 min at rt. The extraction was carried out with EtOAc (2×500 mL) and washed with brine (2×150 mL). The combined organic layers were dried over MgS04, filtered and removed in vacuo. The crude material was purified on silica gel and eluted with EtOAc/hexanes (from 5% to 20%) to yield 1-{[2- (trimethylsilyl)ethoxy]methyl]-1H pyrazole-4-carbaldehyde (12.34 g, 34%) as brown oil

The synthetic route of 2075-45-8 has been constantly updated, and we look forward to future research findings.

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 25016-17-5, name is Methyl 5-methyl-1H-pyrazole-3-carboxylate, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: 25016-17-5

5-methyl-1- (pyrimidin-2-yl-methyl)lH-pyrazole-3-carboxylate (Scheme C-1)5-methyl -1H- pyrazole-3-carboxylate (4.60 g of the) in90mLN, N- dimethylformamideAmine solution and potassium carbonate (10.88g) and themixture is stirred at room temperature for 15 minutes.Then, 2- (chloromethyl) pyrimidine hydrochloride (6.49 gof), and the reaction mixture was heated at reflux18 hours, poured into 300mL water and extracted with ethylacetate. The organic phase was dried with sodium sulfate,Filtered and concentrated under reduced pressure. By columnchromatography on silica gel with cyclohexane / ethyl acetate (1: 9)The crude product was purified as eluent. 0.96g3- givemethyl-1- (pyrimidin-2-ylmethyl) lH-Pyrazole-5-carboxylate and 3.85g of the titlecompoun

According to the analysis of related databases, 25016-17-5, the application of this compound in the production field has become more and more popular.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 1280210-79-8, name is tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-carboxylate, A new synthetic method of this compound is introduced below., HPLC of Formula: C10H15N3O2

Synthesis of 257-A and 258-A. A mixture of tert-butyl 4,6-dihydropyrrolo[3,4- c]pyrazole-5(2H)-carboxylate (314 mg, 1.50 mmol), Cs2CO3 (978 mg, 3.00 mmol) and iodomethane (320 mg, 2.25 mmol) in DMF (6 mL) was stirred at room temperature for 16 h. The mixture was diluted with water (18 mL), extracted with EtOAc (10 mL × 3). The combined organic layer was washed with brine (10 mL × 3), dried over anhydrous Na2SO4 and then concentrated in vacuo. The residue was purified by column chromatography on silica gel (DCM : MeOH = 100 : 1 ~ 50 : 1) to give 257-A and 258-A (270 mg, 81%) as a yellow solid.

The synthetic route of 1280210-79-8 has been constantly updated, and we look forward to future research findings.