HRID1494667

反应详情

EQUATION

反应方程式

HRID 1494667 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Mercaptomethyl-2-n-propylpropan-1,3-dithiol (4.0 g.) and triethyl orthoformate (3.6 g.) were refluxed, with stirring, in dry benzene (120 ml.) containing Amberlyst "15" (1.0 g.). The mixture was cooled and filtered. The filtrates were evaporated in vacuo and the residue was purified by chromatography on alumina eluting with 1:10, dichloromethane: hexane saturated with ammonia. 4-n-Propyl-2,6,7-trithiabicyclo[2.2.2]octane was obtained as a colourless solid (3.1 g., m.pt. 139°).

WORKUP

后处理

  1. additioncontaining Amberlyst "15" (1.0 g.)
  2. temperatureThe mixture was cooled
  3. filtrationfiltered
  4. customThe filtrates were evaporated in vacuo
  5. customthe residue was purified by chromatography on alumina eluting with 1:10, dichloromethane