HRID1702522

反应详情

EQUATION

反应方程式

HRID 1702522 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of 10.8 g (0.2 mol) of sodium methoxide in 70 ml of methanol at room temperature was added dropwise 12 ml (10.8 g, 0.22 mol) of methyl mercaptan through a gas addition funnel connected to a dry-ice condenser. The resulting mixture was stirred at room temperature for 1 hour and then added dropwise to a stirred solution of 30.0 g (0.175 mole) of o-nitrobenzyl chloride in 120 ml of methanol over 1 hour, while the temperature rose to 40° C. The reaction mixture was then diluted with 300 ml of water, and extracted 3 times with methylene chloride. The methylene chloride extracts were washed with dilute hydrochloric acid, dried, and concentrated to afford 38.6 g (96%) of yellow oil.

WORKUP

后处理

  1. additionthrough a gas addition funnel
  2. customconnected to a dry-ice condenser
  3. customrose to 40° C
  4. extractionextracted 3 times with methylene chloride
  5. washThe methylene chloride extracts were washed with dilute hydrochloric acid
  6. customdried
  7. concentrationconcentrated