HRID927197

反应详情

EQUATION

反应方程式

HRID 927197 的结构方程式

PROCEDURE

实验过程

A solution of hydrogen chloride in 1,4-dioxane (4 M, 29.3 mL, 117 mmol) is added to a mixture of tert-butyl(4-cyanophenyl)(5-oxo-2-(3-(trifluoromethyl)phenylamino)cyclopent-1-enyl)methylcarbamate (intermediate 12, 6.92 g, 14.7 mmol) in 1,4-dioxane (30 mL), and the mixture is stirred at room temperature for 2 h. All volatiles are removed under reduced pressure, and the residue is treated with tert-butyl methyl ether (50 mL). The precipitate is filtered, washed with tert-butyl methyl ether and dried. Yield: 6.10 g. ESI mass spectrum: [M+H]+=372; Retention time HPLC: 0.62 min (X011_S02).

WORKUP

后处理

  1. customAll volatiles are removed under reduced pressure
  2. additionthe residue is treated with tert-butyl methyl ether (50 mL)
  3. filtrationThe precipitate is filtered
  4. washwashed with tert-butyl methyl ether
  5. customdried
  6. custom0.62 min (X011_S02)