HRID256287

反应详情

EQUATION

反应方程式

HRID 256287 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
16 °C

PROCEDURE

实验过程

To a chilled solution of 1.12 g (0.0098 mole) of tetrahydrothiophene-3-ol in 15 mL of pyridine was added 1.91 g (0.01 mole) of 4-methylphenylsulfonyl chloride, and the reaction mixture was stirred in the cold, about 16° C., for 1 hour then placed in a cold refrigerator for 16 hours. The reaction mixture was allowed to warm to room temperature and was stirred for 1 hour. An additional 0.3 g (0.0016 mole) of 4-methylphenylsulfonyl chloride was added, and the reaction mixture was stirred at room temperature for 64 hours. The reaction mixture was poured into water, and the whole was extracted with methylene chloride. The methylene chloride solution was dried and concentrated to give 1.28 g of product as an oil.

WORKUP

后处理

  1. temperatureto warm to room temperature
  2. stirringwas stirred for 1 hour
  3. stirringthe reaction mixture was stirred at room temperature for 64 hours
  4. extractionthe whole was extracted with methylene chloride
  5. dry with materialThe methylene chloride solution was dried
  6. concentrationconcentrated