Tag: M.W:100-200

Reference of 402-61-9, These common heterocyclic compound, 402-61-9, name is 5-Methyl-1H-pyrazole-3-carboxylic acid, 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.

A solution of 4.30 g (34.1 mmol) of 5-methyl-1H-pyrazole-3-carboxylic acid in 20 ml of anhydrous DMF was added dropwise at RT within approx. 15 min to a suspension of 5.81 g (35.8 mmol) of 1,1′-carbonyldiimidazole (CDI) in 25 ml of anhydrous DMF. After the mixture had been stirred at RT for 105 min, 8.12 g (34.1 mmol) of the compound from Example 5A/Step 3 were added. Subsequently, the reaction mixture was heated to 110 C. for 5 h. After cooling to RT, the mixture was stirred gradually into 800 ml of water. In the course of this, the product precipitated out. It was filtered off with suction and washed with water. Subsequently, the moist crude product was recrystallized from 430 ml of ethanol. After the solid had been filtered and dried, 8.31 g (74% of theory) of the title compound were obtained. A further fraction was obtained by concentrating the mother liquor (1.69 g with 85% purity, 13% of theory).1H NMR (400 MHz, CDCl3, delta/ppm): 10.73 (broad, 1H), 8.20 (d, 2H), 7.52 (d, 2H), 6.81 (s, 1H), 4.00-3.88 (m, 4H), 2.45 (s, 3H), 2.30-2.11 (m, 2H), 1.98-1.91 (m, 2H).LC/MS (method 1, ESIpos): Rt=4.24 min, m/z=329 [M+H]+.

Statistics shows that 5-Methyl-1H-pyrazole-3-carboxylic acid is playing an increasingly important role. we look forward to future research findings about 402-61-9.

Reference of 16034-46-1,Some common heterocyclic compound, 16034-46-1, name is 1-Methyl-1H-pyrazole-5-carboxylic acid, molecular formula is C5H6N2O2, 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.

Oleum (1977mmol) is slowly added to fuming nitric acid (777 mmol) followed by the addition of 2-methyl-2H-pyrazole-3-carboxylic acid (277 mmol) in small portions maintaining the reaction temperature below 6O0C. Stirring at this temperature is then continued for a further 1 h. On completion, the reaction mixture is poured onto crushed ice and extracted with ethyl acetate (300 mL x 3). The combined organic phases are washed with water (250 mL x 2) and dried over anhydrous sodium sulfate. The solvent is removed under reduced pressure to afford 2-methyl-4-nitro-2H-pyrazole-3- carboxylic acid as a light yellow solid. Compound wt: 23.6g, 50%.[00251] 1H NMR (400 MHz, OMSO-d6) delta: 8.29 (lH,s); 3.95 (3H, s).

The synthetic route of 16034-46-1 has been constantly updated, and we look forward to future research findings.

Some common heterocyclic compound, 82560-12-1, name is 3-Amino-5-tert-butylpyrazole, molecular formula is C7H13N3, 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. Recommanded Product: 82560-12-1

Step j04: 3-Tert-butyl-1H-pyrazol-5-amine (J-III) (1 eq., 40 g) was dissolved in dilute HCl (120 ml of HCl in 120 ml of water) and mixed dropwise with NaNO2 (1.03 eq., 25 g in 100 ml) at 0-5 C. over a period of 30 min. After stirring for 30 minutes, the reaction mixture was neutralised with Na2CO3. A diazonium salt obtained by reaction of KCN (2.4 eq., 48 g), water (120 ml) and CuCN (1.12 eq., 31 g) was added dropwise to the reaction mixture within 30 min and the mixture was stirred for a further 30 min at 75 C. After complete reaction, the reaction mixture was extracted with EE (3×500 ml), the combined organic phases were dried over sodium sulphate and the solvent was removed under vacuum. The purification (SiO2, 20% EE/hexane) of the residue by column chromatography produced a white solid (J-IV) (6.5 g, 15.1% yield).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 82560-12-1, its application will become more common.

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. 133228-21-4, name is N,N-Dimethyl-1H-pyrazole-1-sulfonamide, A new synthetic method of this compound is introduced below., COA of Formula: C5H9N3O2S

N,N-dimethyl-lH-pyrazole-l -sulfonamide (8.89 g, 50.8 mmol) was dissolved in anhydrous THF (250 mL). The solution was cooled at -78C, a solution of n-butyl lithium (32.6 mL, 81.4 mmol, 2.5 M in hexane) was added dropwise, and then the mixture was stirred for 45 minutes. A solution of hexachloroethane (18.0 g, 76.3 mmol) in anhydrous THF (20 mL) was added dropwise at -78C, and the reaction stirred for 1.5 hours. Water was added, and the mixture was extracted 5 times with dichloromethane. The combined organic phases were washed with brine and then dried over magnesium sulfate. After evaporation of the solvent, 5-chloro-N,N- dimethyl-lH-pyrazole-1 -sulfonamide was obtained and used in the next step without further purification.

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.

Synthetic Route of 1126-00-7, The chemical industry reduces the impact on the environment during synthesis 1126-00-7, name is 1-Phenylpyrazole, I believe this compound will play a more active role in future production and life.

EXAMPLE 29A 4-Bromo-1-phenyl-1H-pyrazole To 1-phenylpyrazole (Aldrich, 1 g, 6.94 mmol) in 10 mL acetic acid was added 1.1 g of Br2 (Fisher, 6.94 mmol) in 10 mL acetic acid. This mixture was warmed to 100 C. in a pressure tube for 8 h. The material was cooled to ambient temperature, poured into ice and H2O in a 500 mL beaker and excess saturated, aqueous NaHCO3 was added until all the acetic acid had been quenched. EtOAc (50 mL) was added and the layers were separated. The aqueous layer was extracted 2*15 mL EtOAc and the combined organics were dried over Na2SO4 and concentrated under reduced pressure to give a crude solid. Purification via flash column chromatography (SiO2, 50% hexanes-EtOAc) gave 1.5 g of the title compound (6.72 mmol, 97% yield). MS (DCI/NH3) m/z 223, 225 (M+H)+.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 1-Phenylpyrazole, other downstream synthetic routes, hurry up and to see.

Application of 5775-86-0, These common heterocyclic compound, 5775-86-0, name is 4-Bromo-1,5-dimethylpyrazole, 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.

To a solution of tert-butyl (3S)-3-[[4-[1-(benzenesulfonyl)-6-(4,4,5,5-tetramethyl]-1,3,2-dioxaborolan-2-yl)indol-3-yl]-5-(trifluoromethyl)pyrimidin-2-yl]amino]piperidine-1-carboxylate (120.00 mg, 164.93 umol) and 4-bromo-1,5-dimethyl-pyrazole (31.75 mg, 181.42 umol) in dioxane (5 mL) and H2O (500 uL) was added Pd(PPh3)4 (19.06 mg, 16.49 umol) and Cs2CO3 (107.47 mg, 329.85 umol). The mixture was stirred at 100 C for 4 h under N2. The mixture was poured into water (100 mL). The aqueous phase was extracted with EA (50 mL*3). The combined organic phase was washed with brine (100 mL), dried with anhydrous Na2SO4, filtered and concentrated. The residue was purified by column chromatography (SiO2, Petroleum ether/ethyl acetate=5/1 to 2:1) to give to afford the title compound (150 mg, crude).

Statistics shows that 4-Bromo-1,5-dimethylpyrazole is playing an increasingly important role. we look forward to future research findings about 5775-86-0.

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. 400877-57-8, name is Methyl 1-methyl-4-nitro-1H-pyrazole-3-carboxylate, A new synthetic method of this compound is introduced below., Quality Control of Methyl 1-methyl-4-nitro-1H-pyrazole-3-carboxylate

240 mg (1.30 mM) of the compound obtained in Preparative Example 7 was dissolved in 5 ml of methanol, to which 24 mg of 10% palladium/ EPO charcoal was added dropwise, and the resulting mixture was stirred under hydrogen pressure of 40 atm for 30 minutes. After the reaction was terminated, the resulting reaction solution was filtered through cellite, and distilled under reduced pressure, to obtain 191 mg (95%) of the title compound.1H NMR(SOOMHZ, CDCl3) delta 3.86(s, 3H), 3.92(s, 3H), 6.91(s, IH). Mass : 155(M+)

The synthetic route of 400877-57-8 has been constantly updated, and we look forward to future research findings.

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 449758-17-2 as follows. name: 1-(2-Tetrahydropyranyl)-1H-pyrazole

Preparation 2 6-[1-Hydroxy-1-(1-tetrahydropyran-2-yl-1H-pyrazol-5-yl)ethyl]-3-(methoxymethyl)-3H-1,3-benzothiazol-2-one (Racemic mixture of diasteromers) Add 1-tetrahydropyran-2-yl-pyrazole (1.5 Eq, 202 mmoles, 30.8 g)(Aldrich) and THF (900 mL) to a flame dried 2 L 3 neck round bottom flask and cool to -78 C. (dry ice/acetone bath). Add t-butyl lithium (2.5 M in THF)(1.5 Eq, 202 mmoles; 81.0 mL) dropwise, maintaining at least -68 C., and stir for 60 min at -78 C. Add a solution of 6-acetyl-3-(methoxymethyl)-3H-1,3-benzothiazol-2-one (32.0 g, 134 mmoles) in THF (450 mL) dropwise over 45 min, and stir at -78 for 30 min. Remove the dry ice bath and allow to warm to -50 C. and stir for 1 hr. (do not let temp. rise above -45 C.). Quench the reaction with MeOH (80 mL). Transfer to a separatory funnel, add EtOAc (2000 mL), and wash with water (500 mL) and then brine (500 mL). The organic layer is dried over Na2SO4, filter and concentrate to give a crude yellow oil. Purify the material by HPLC, eluting with hexanes/EtOAc (6:4) to yield 6-[1-hydroxy-1-(1-tetrahydropyran-2-yl-1H-pyrazol-5-yl)ethyl]-3-(methoxymethyl)-3H-1,3-benzothiazol-2-one as a white foam (44 g, 113 mmoles, 84% yield) (Racemic mixture of diasteromers). LCMS (Low) rt=1.76 min., M+1=288, and rt=1.86 min., M+1=288

According to the analysis of related databases, 449758-17-2, the application of this compound in the production field has become more and more popular.

Electric Literature of 288148-34-5,Some common heterocyclic compound, 288148-34-5, name is 1-Methyl-1H-pyrazole-4-sulfonyl chloride, molecular formula is C4H5ClN2O2S, 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.

100 mg (0.25 mmol) of 2-(4-benzyl-3-(ethoxycarbonylamino)chroman-6- yloxy)ethanaminium chloride were dissolved in 5 ml methylene dichloride. Then, 95 mg (0.79 mmol) dimethyl aminopyridine and 54 mg (0.30 mmol) 1 -methyl-1 H-pyrazole-4- sulfonyl chloride were added. The reaction mixture was stirred at room temperature over night. The mixture was concentrated in vacuo and the residue was dissolved in ethylace- tate and water. The phases were separated. The organic phase was washed with saturated ammonium chloride solution (2x), dried over MgS04 and concentrated (127 mg crude). The crude material was purified by column chromatography to give 1 18 mg (0.23 mmol, 93 %) of the desired product.ESI-MS [M+H+] = 515 Calculated for C25H3oN406S = 514.

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-1H-pyrazole-4-sulfonyl chloride, its application will become more common.

Electric Literature of 75415-03-1, A common heterocyclic compound, 75415-03-1, name is 2-(1H-Pyrazol-3-yl)pyridine, molecular formula is C8H7N3, 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.

To a solution of 3-(2-pyridyl)pyrazole (291 mg, 2 mmol) in THF (20 mL) was added NaH (0.3 g, 12.5 mmol). The mixture was stirred for lh and the Mel (568 mg, 4 mmol) was added in one portion. The reaction mixture was stirred for 18h at room temperature. The reaction was quenched with MeOH and the solvent was removed in vacuo. The residue was treated with water and EtOAc. The organic layer was separated and the aqueous layer was extracted with EtOAc. The combined organic phase was dried over Na2S04, filtered, and concentrated to give crude product. The crude product was purified on ISCO columns. Fractions containing pure product were combined and evaporated to give 3-(2-pyridyl)-l-methylpyrazole (300 mg, 94%) as a yellow oil.

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.