The origin of a common compound about 1145-01-3

The synthetic route of 3,5-Diphenyl-1H-pyrazole has been constantly updated, and we look forward to future research findings.

A common heterocyclic compound, 1145-01-3, name is 3,5-Diphenyl-1H-pyrazole, molecular formula is C15H12N2, 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. 1145-01-3.

EXAMPLE 5 The preparation of 1 -methyl-3,5-diphenylpyrazole Five parts of 3,5-diphenylpyrazole are dissolved in 25 parts (by volume) of methyl isobutyl ketone. Solid anhydrous sodium hydroxide (1.1 parts) is added and the mixture is heated to 90C. Dimethyl sulfate (3.43 parts) is added and the mixture is next heated to 112C. to 115C. The reaction mixture is sampled after 1.5 hours, and no unreacted 3,5-diphenylpyrazole is found to be present. The reaction mixture is cooled to 50C., and 30 parts of water are added. The pH is next adjusted to between 11 and 12 by the addition of aqueous sodium hydroxide. The organic layer is washed twice with 30 parts water. For yield determination the methyl isobutyl ketone is removed in vacuo, producing 4.95 parts (93% crude yield) of an oil which crystallizes on cooling (melting point 52C. to 53C). Analysis of the product shows it to be 85.5% pure as 1-methyl-3,5-diphenylpyrazole.

The synthetic route of 3,5-Diphenyl-1H-pyrazole has been constantly updated, and we look forward to future research findings.

Share a compound : 3,5-Diphenyl-1H-pyrazole

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, 3,5-Diphenyl-1H-pyrazole, other downstream synthetic routes, hurry up and to see.

1145-01-3, A common compound: 1145-01-3, name is 3,5-Diphenyl-1H-pyrazole, belongs to pyrazoles-derivatives compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below.

Potassium hydroxide (0.800 g, 14 103 mol) was treated with 9.0 mL of DMSO and the resulting mixture was magnetically stirred at room temperature (ca. 298 K) for 30 min. After this period 3,5-diphenylpyrazole (0.788 g, 3.58 103 mol) was added and the stirring was maintained for 30 min at 298 K. Then, 1-chloro-2-methoxyethane (4.0 mL, 45 103 mol) was gradually added and the reaction mixture was left overnight under stirring at 298 K. After this period, 50 mL of iced cold water was added to eliminatethe unreacted KOH; the organic phase was then extracted with diethylether and washed repeatedly with water, dried over Na2SO4 and filtered. Then, the filtrate was concentrated to dryness on arotary evaporator. The solid formed was collected and later on dried in vacuum for 3 days. [Yield: 0.880 g, (88%)]. Characterization data:Anal (%). Calc. for C18H18N2O (MW 278.35): C, 77.67; H, 6.52; N,10.06%; found: C, 77.8; H, 6.6 and N, 10.1. MS (ESI): m/z 279.15{[M] H}. IR selected data: 3059-3015 [n(CeH)] and 2987-2952[n(CeH)], 1481(m), 1462(s), 1441(m), 1363(m), 1300(m), 1115(s),1012(m), 762(s), 691(s) cm1. UV-vis data (c 5.74 x 10-5 M in CH2Cl2): l (epsilon) 223 (1.5 104) and 253 (3.1 104). Rf (inCHCl3) 0.24. 1H NMR data: d 3.32 (s, 3H, OMe); 3.91 [t,3JH,H 7.2, 2H, (-CH2-d)]; 4.34 [t, 3JH,H 7.2, 2H, (-CH2-c)]; 6.65(s, 1H, H4); 7.35 (t, 3JH,H 7.7, 1H, H4b); 7.47e7.60 (m, 5H, H3a, H4a,H5a, H3b and H5b); 7.70 (d, 2H, 3JH,H 7.6, H2b and H6b), 7.92 (d, 2H,3JH,H 7.5, H2a and H6a). 13C{1H} NMR data: 49.1 (Cd); 58.9 (OMe);71.4 (Cc); 103.4 (C4); 125.3 (C2b and C6b); 125.7 (C2a and C6a); 126.0(C4b); 126.8 (C4a); 128.7 (C3a and C5a); 129.2 (C3b and C5b); 130.7(C1b); 133.6 (C1a); 145.9 (C5) and 150.9 (C3).

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, 3,5-Diphenyl-1H-pyrazole, other downstream synthetic routes, hurry up and to see.