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HRID377695

反应详情

EQUATION

反应方程式

HRID 377695 的结构方程式

REACTANTS

反应物

4
结构：C=CCBr
HCID7841

Allyl bromide

C3H5Br

结构：O=C([O-])[O-].[K+].[K+]
HCID11430

Potassium Carbonate

CK2O3

结构：CS(=O)(=O)c1ccc(-c2n[nH]c(C(F)(F)F)c2-c2ccc(F)cc2)cc1
HCID15380222

未命名化合物

结构：C=CCn1nc(C(F)(F)F)c(-c2ccc(F)cc2)c1-c1ccc(S(C)(=O)=O)cc1
HCID19355906

未命名化合物

PRODUCTS

生成物

1
结构：C=CCn1nc(-c2ccc(S(C)(=O)=O)cc2)c(-c2ccc(F)cc2)c1C(F)(F)F
HCID9954100

未命名化合物

收率 41%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CN(C)C=O
溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

PROCEDURE

实验过程

Reaction of 4-(4-fluorophenyl)-3-[4-(methylsulfonyl)phenyl]-5-(trifluoromethyl)-1H-pyrazole (Example 1, Step 3) (0.1 g) with 0.08 g of potassium carbonate and 2.0 g of allyl bromide in 5 mL of DMF gave a crude mixture of 1-allyl-4-(4-fluorophenyl)-5-[4-(methylsulfonyl)phenyl]-3-(trifluoromethyl)pyrazole and 1-allyl-4-(4-fluorophenyl)-3-[4-(methylsulfonyl)phenyl]-5-5 (trifluoromethyl)-1H-pyrazole. HPLC purification with 50% ethyl acetate-hexane and recrystallization from ether-hexane gave 1-allyl-4-(4-fluorophenyl)-3-[4-(methylsulfonyl)phenyl]-5-(trifluoromethyl)-1H-pyrazole (45 mg, 41%): mp 115.5-119° C.

WORKUP

后处理

  1. customgave a crude
  2. customHPLC purification
  3. customwith 50% ethyl acetate-hexane and recrystallization from ether-hexane