HRID59088

反应详情

EQUATION

反应方程式

HRID 59088 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of (2-chloro-6-(1-ethoxyvinyl)pyrimidin-4-yl)methyl methanesulfonate (0.452 g, 1.54 mmol) in benzene (7 mL) were added 3,3,3-trifluoropropan-1-ol (0.264 g, 2.32 mmol), sodium hydroxide (5 M, 0.463 mL, 2.32 mmol) and tetrabutylammonium hydrogen sulfate (0.052 g, 0.15 mmol). The mixture was stirred vigourously over night at room temperature. The mixture was filtered through a short silica plug with magnesium sulfate on top. The filter was washed with EtOAc. The mixture was purified by preparative HPLC to give 2-chloro-4-(1-ethoxyvinyl)-6-((3,3,3-trifluoropropoxy)methyl)pyrimidine 0.055 g 11%).

WORKUP

后处理

  1. filtrationThe mixture was filtered through a short silica plug with magnesium sulfate on top
  2. washThe filter was washed with EtOAc
  3. customThe mixture was purified by preparative HPLC