HRID1594877

反应详情

EQUATION

反应方程式

HRID 1594877 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To a solution of 2-fluoro-4-(hydroxy-pyridin-3-yl-methyl)-benzonitrile (as described in Example 20, Step C) (0.4 g, 1.75 mmol) in CH2Cl2 (25.0 mL) at 0° C. was added phenyl thionochloroformate (0.388 mL, 2.8 mmol) and DMAP (0.471 g, 3.86 mmol). The solution was stirred at 25° C. for 3 hr. The reaction was partitioned with saturated NaHCO3 and CH2Cl2. The CH2Cl2 layer was washed with brine, dried with MgSO4, and evaporated in vacuo to obtain the title compound after chromatography (silica gel, CH2Cl2:MeOH 99:1).

WORKUP

后处理

  1. customThe reaction was partitioned with saturated NaHCO3 and CH2Cl2
  2. washThe CH2Cl2 layer was washed with brine
  3. dry with materialdried with MgSO4
  4. customevaporated in vacuo