HRID333558

反应详情

EQUATION

反应方程式

HRID 333558 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N2-phenylpyridine-2,3-diamine (14.1 g, 76 mmol) and acetone (8.39 mL, 114 mmol) was added to a solution of acetic acid and dichloromethane. Sodium triacetoxyborohydride (22.59 g, 107 mmol) was added to the reaction mixture and stirred overnight at room temperature. Reaction mixture was quenched with 1N HCl. Organic layer was extracted with ethyl acetate. Ethyl acetate solution was washed with 1N sodium hydroxide solution followed by brine and dried over anhd. MgSO4. N3-isopropyl-N2-phenylpyridine-2,3-diamine (16.3 g, 94% yield) was isolated from crude by column chromatography using hexanes and ethyl acetate as eluent.

WORKUP

后处理

  1. customReaction mixture
  2. customwas quenched with 1N HCl
  3. extractionOrganic layer was extracted with ethyl acetate
  4. washEthyl acetate solution was washed with 1N sodium hydroxide solution
  5. customdried over anhd