HRID725000

反应详情

EQUATION

反应方程式

HRID 725000 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Thiourea (0.29 g) and 4,4-difluorobut-3-enyl 4-methyl-benzenesulfonate (1 g) were heated together under reflux in ethanol (20 cm3) for 24 hours. The reaction mixture was cooled and the solvent evaporated under reduced pressure to give an oil which slowly crystallised. Trituration with hexane gave (4,4-difluorobut-3-enyl)-thiourea as its 4-methyl-benzenesulfonate salt (1.14 g). MH+ (FAB)=167; 1H NMR (DMSO-d6): δ 2.48(3H,s); 2.46-2.58(2H,m); 3.42(2H,t); 4.66-4.84(1H,m); 7.32(2H,d); 7.68(2H,d); 9.10-9.40(3H,br)

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. customthe solvent evaporated under reduced pressure
  3. customto give an oil which
  4. customslowly crystallised