HRID1060880

反应详情

EQUATION

反应方程式

HRID 1060880 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

2-Fluoro-4-(3-methyl-3H-imidazole-4-carbonyl)-benzonitrile (2.56 g, 11.2 mmol), titanium(IV) ethoxide (7.02 mL, 33.5 mmol) and commercially available (R)-(+)-2-methyl-2-propanesulfinamide (1.35 g, 11.17 mmol) were dissolved in anhydrous THF (100 mL) and heated at 75° C. for 7 days. The solution was cooled, diluted with brine (100 mL), filtered through a celite pad and washed generously with EtOAc and H2O. The filtrate was separated, dried (MgSO4), and purified using SiO2 chromatography (0-3% MeOH/CH2Cl2) to give the title compound.

WORKUP

后处理

  1. temperatureThe solution was cooled
  2. filtrationfiltered through a celite pad
  3. washwashed generously with EtOAc and H2O
  4. customThe filtrate was separated
  5. dry with materialdried (MgSO4)
  6. custompurified