HRID3922

反应详情

EQUATION

反应方程式

HRID 3922 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of 2-amino-4-trifluoromethylthiophenol hydrochloride (30.0 g) in ethanol (125 ml) was added 2-chloro-1,1,1-triethoxyethane (31.0 g). The mixture was heated for 1 hour at 60° C. The solution was concentrated to remove excess ethanol and the resulting material was extracted with ether (500 ml). The organic extract was washed successively with 10% HCl (20 ml), water (100 ml), 10% sodium bicarbonate solution and water (100 ml), and then evaporated to obtain an amber colored oil, which crystallized upon standing at room temperature (28.9 g; m.p. 52° C).

WORKUP

后处理

  1. concentrationThe solution was concentrated
  2. customto remove excess ethanol
  3. extractionthe resulting material was extracted with ether (500 ml)
  4. extractionThe organic extract
  5. washwas washed successively with 10% HCl (20 ml), water (100 ml), 10% sodium bicarbonate solution and water (100 ml)
  6. customevaporated
  7. customto obtain an amber colored oil, which
  8. customcrystallized
  9. customupon standing at room temperature