HRID502602

反应详情

EQUATION

反应方程式

HRID 502602 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

A mixture of 2-chloro-6-methylbenzonitrile (3.00 g, 19.80 mmol), and sodium thiomethoxide (2.91 g, 41.58 mmol) in 1-methyl-2-pyrrolidinone (25 mL) was heated at 140° C. overnight. The reaction mixture was cooled to 0° C. and quenched with 50% aqueous HCl. A light yellow precipitate formed and the reaction was cooled for 1 h while stirring. The yellow solid was collected by vacuum filtration, washed with ice-cold water and dried under reduced pressure overnight to provide 2-mercapto-6-methylbenzonitrile (1.0 g). The crude product was carried forward without further purification. MW=149 confirmed by LC-MS, tr=2.98 min (Method E) MH+=150.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to 0° C.
  2. customquenched with 50% aqueous HCl
  3. customA light yellow precipitate formed
  4. temperaturethe reaction was cooled for 1 h
  5. filtrationThe yellow solid was collected by vacuum filtration
  6. washwashed with ice-cold water
  7. customdried under reduced pressure overnight