HRID584239

反应详情

EQUATION

反应方程式

HRID 584239 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Acetic acid (5.4 ml) was added to a solution of 2-amino-2-methyl-1-propanol (8.4 g) and benzaldehyde (10 g) in 1,2-dichloroethane (140 ml) under ice-cooling. After 30 minutes of stirring at the same temperature, sodium triacetoxyborohydride (26 g) was added by small portions to the solution over 10 minutes. After 2 hours of stirring at room temperature, the mixture was poured into a solution of sodium hydrogen carbonate (48 g) in water (300 ml). The aqueous layer was separated and adjusted to pH 12 with 24% sodium hydroxide aqueous solution. The alkaline solution was extracted with ethyl acetate (2 times). The extract was dried over sodium sulfate and evaporated under reduced pressure to give colorless crystals of 2-benzylamino-2-methyl-1-propanol (13.2 g).

WORKUP

后处理

  1. temperaturecooling
  2. additionwas added by small portions to the solution over 10 minutes
  3. customThe aqueous layer was separated
  4. extractionThe alkaline solution was extracted with ethyl acetate (2 times)
  5. dry with materialThe extract was dried over sodium sulfate
  6. customevaporated under reduced pressure