HRID1264196

反应详情

EQUATION

反应方程式

HRID 1264196 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-5 °C

PROCEDURE

实验过程

A solution of 4-(2-tert-butoxy-phenylamino)-2-chloro-2′-methylbenzophenone (Compound 107) (1.33 g, 3.4 mmol) in a mixture of CH2Cl2 (5 ml) and trifluoroethanol (20 ml) was cooled to −5° C. under argron. Trifluoroacetic acid (423 mg, 3.7 mmol) was added dropwise and the reaction mixture was allowed to come to room temperature over 1 h. After 23 h at room temperature the reaction mixture was poured into saturated NaHCO3 and then extracted with EtOAc and CH2Cl2. The organic phases was collected, dried (MgSO4), filtered, and concentrated in vacuo to give the crude product. This was further purified by flash chromatography using EtOAc/pentane 1:4 as eluant.

WORKUP

后处理

  1. extractionextracted with EtOAc and CH2Cl2
  2. customThe organic phases was collected
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo