HRID2107369

反应详情

EQUATION

反应方程式

HRID 2107369 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of nitropropane (0.45 g, 0.005 moles) in dichloromethane (25 mL) at 0° C. was added triethylamine (0.67 mL, 0.005 moles) followed by ethyl aluminum dichloride (1.0 M in hexane, 5 mL, 0.005 moles). After 15 minutes benzaldehyde (0.5 mL 0.005 moles) was added and the solution allowed to warm to room temperature. After a further 3 hours the reaction was cooled in ice to a temperature of 5° C. and quenched with pH 7.0 phosphate buffer. The organic layer was separated, dried and evaporated in vacuo. Flash column chromatography [SiO2, 6:1 hexane, Et2O] gave 1-phenyl-2-nitro-1-butanol (0.28 g, 29%) Erythro:threo ratio 1:1.6.

WORKUP

后处理

  1. temperatureAfter a further 3 hours the reaction was cooled in ice to a temperature of 5° C.
  2. customquenched with pH 7.0 phosphate buffer
  3. customThe organic layer was separated
  4. customdried
  5. customevaporated in vacuo