HRID1870553

反应详情

EQUATION

反应方程式

HRID 1870553 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A mixture of 4-(trifluoromethyl)benzamidine hydrochloride dihydrate (5.0 g), water (50 mL), methylene chloride (100 mL), benzyltriethylammonium chloride (0.44 g), and perchloromethyl mercaptan (2.1 mL) was prepared at room temperature and then cooled to 0° C. A solution of sodium hydroxide (3.07 g) in water (50 mL) was added via an addition funnel while maintaining the temperature below 10° C. The reaction was left to stir overnight at room temperature. The mixture was transferred to a separatory funnel and the two layers were separated. The organic layer was washed with saturated sodium bicarbonate, dried (MgSO4), filtered and concentrated under reduced pressure. The crude material was purified by flash chromatography (hexane as eluent) to afford 3.7 g of the title compound of Step H as a white powder. 1H NMR (CDCl3): δ 8.36 (d,2H), 7.73 (d,2H).

WORKUP

后处理

  1. customwas prepared at room temperature
  2. temperaturewhile maintaining the temperature below 10° C
  3. waitThe reaction was left
  4. customThe mixture was transferred to a separatory funnel
  5. customthe two layers were separated
  6. washThe organic layer was washed with saturated sodium bicarbonate
  7. dry with materialdried (MgSO4)
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure
  10. customThe crude material was purified by flash chromatography (hexane as eluent)