HRID59653

反应详情

EQUATION

反应方程式

HRID 59653 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

{(2-Bromo-4-cyano-phenyl)-[6-oxo-2-(3-trifluoromethyl-phenylamino)-cyclohex-1-enyl]-methyl}-carbamic acid tert-butyl ester (INTERMEDIATE 20, 20.8 g, 36.9 mmol) is suspended in acetonitrile (150 mL) and a solution of hydrogen chloride in 1,4-dioxane (4 M, 46.1 mL, 184.3 mmol) is added. The mixture is stirred at room temperature for 3 h. The product precipitates from the reaction mixture. The precipitate is filtered off, washed with acetonitrile and dried. Yield: 16.5 g ESI mass spectrum: [M+H]+=464 (bromine isotope pattern), Retention time HPLC: 0.56 min, (X012_S02).

WORKUP

后处理

  1. customThe product precipitates from the reaction mixture
  2. filtrationThe precipitate is filtered off
  3. washwashed with acetonitrile
  4. customdried
  5. custom0.56 min, (X012_S02)