HRID270927

反应详情

EQUATION

反应方程式

HRID 270927 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1.97 g (15.5 mmol) of tetrahydro-thiopyran-4-carbonitrile in 5 mL of ethanol (EtOH) was added to a solution of 6.2 g (155 mmol) of sodium hydroxide (NaOH) in 30 mL of EtOH and 15 mL of water, and the resulting mixture was heated at reflux for 4 h. The reaction mixture was cooled in an ice bath, acidified with concentrated hydrochloric acid to pH=2, and then concentrated to give a precipitate which was filtered to afford 1.36 g (60%) of desired tetrahydro-thiopyran-4-carboxylic acid as a brown crystalline solid as indicated by 1H NMR.

WORKUP

后处理

  1. temperaturethe resulting mixture was heated
  2. temperatureat reflux for 4 h
  3. temperatureThe reaction mixture was cooled in an ice bath
  4. concentrationconcentrated
  5. customto give a precipitate which
  6. filtrationwas filtered