HRID724965

反应详情

EQUATION

反应方程式

HRID 724965 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2-chloro-5,11-dihydro-11-ethyl-8-formyl-5-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one (0.5822 g, 1.84 mmol) in tetrahydrofuran (20 mL) was added water (0.1 mL) followed by sodium borohydride (0.0695 g, 1.84 mmol). The mixture was stirred for 0.5 hour then diluted with brine (20 mL) and extracted with dichloromethane (3×30 mL). The combined organics were dried, concentrated and the residue was purified by flash chromatography (gradient hexanes to ethyl acetate to yield the title compound (0.52 g, 89%), m.p. 166°-168° C.

WORKUP

后处理

  1. extractionextracted with dichloromethane (3×30 mL)
  2. customThe combined organics were dried
  3. concentrationconcentrated
  4. customthe residue was purified by flash chromatography (gradient hexanes to ethyl acetate