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HRID430472

反应详情

EQUATION

反应方程式

HRID 430472 的结构方程式

REACTANTS

反应物

5
结构：Cl
HCID313

Hydrochloric Acid

ClH

结构：O=C([O-])[O-].[K+].[K+]
HCID11430

Potassium Carbonate

CK2O3

结构：[H-].[Na+]
HCID24758

Sodium hydride

HNa

结构：CC(=O)Nc1ccc2c(c1)COC2=O
HCID590968

未命名化合物

结构：COc1ccc(F)cc1C(C)CC(O)(COS(=O)(=O)c1ccc(C)cc1)C(F)(F)F
HCID18350645

未命名化合物

PRODUCTS

生成物

1
结构：COc1ccc(F)cc1C(C)(C)CC(C)(O)CNc1ccc2c(c1)COC2=O
HCID18350657

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CN(C)C=O
溶剂HCID6228

N,N-Dimethylformamide

C3H7NO

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

688 mg of 5-acetamidophthalide in 15 ml of dimethylformamide is mixed under argon at 0° C. with 108 mg of an 80% sodium hydride/oil suspension. After 10 minutes of stirring at this temperature, 556 mg of 4-toluenesulfonic acid-[2-hydroxy-4-(5-fluoro-2-methoxyphenyl)-2-trifluoromethyl-pentyl]-ester is added. After 16 hours of stirring at 60° C., it is added to 1 M hydrochloric acid, neutralized with potassium carbonate and extracted with ethyl acetate. After drying (Na2SO4), the crude product is chromatographed on silica gel. With hexane/ethyl acetate (60:40), the title compound is obtained in a crystalline state, flash point 148-149° C.

WORKUP

后处理

  1. additionis added
  2. extractionextracted with ethyl acetate
  3. dry with materialAfter drying (Na2SO4)
  4. customthe crude product is chromatographed on silica gel