HRID892249

反应详情

EQUATION

反应方程式

HRID 892249 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 13.0 g (50.5 mmol) (4-allyloxy-phenyl)-methanethiol and 13.5 g (50.5 mmol) toluene-4-sulfonic acid 2-[1,2,3]triazol-1-yl-ethyl ester in 125 ml N,N-dimethylformamide was added under argon at −30° C. 2.42 g (101 mmol) sodium hydride. The mixture was allowed to warm up to room temperature and was stirred under argon for 12 hours. After quenching with 100 ml water, the mixture was diluted with dichloromethane, washed with water, dried and evaporated. Purification on silica after elution with ethyl acetate/heptane 1:1 yielded 12.0 g (86%) 1-[2-(4-allyloxy-benzylsulfanyl)-ethyl]-1H[1,2,3]triazole as slightly yellow oil.

WORKUP

后处理

  1. additionwas added under argon at −30° C
  2. customAfter quenching with 100 ml water
  3. additionthe mixture was diluted with dichloromethane
  4. washwashed with water
  5. customdried
  6. customevaporated
  7. customPurification on silica
  8. washafter elution with ethyl acetate/heptane 1:1