HRID499097

反应详情

EQUATION

反应方程式

HRID 499097 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

To a solution of 6-bromoquinoline (700 mg) in dimethylacetamide (3 ml) was added sodium thiomethoxide (1.9 g, 26.96 mmol). The mixture was heated at 150° C. for 2 hours, then cooled to ambient and diluted with 1M HCl/ethyl acetate. The organic layer was removed and the aqueous layer extracted with further ethyl acetate. The combined extracts were washed with water, then brine, dried (MgSO4), filtered and concentrated. The crude thiol (500 mg) was used directly without further purification; MS ES+, ES− 174.13

WORKUP

后处理

  1. temperaturecooled
  2. customThe organic layer was removed
  3. extractionthe aqueous layer extracted with further ethyl acetate
  4. washThe combined extracts were washed with water
  5. dry with materialbrine, dried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe crude thiol (500 mg) was used directly without further purification