HRID2380252

反应详情

EQUATION

反应方程式

HRID 2380252 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 5,11-dihydro-11-ethyl-6-methanesulfonyloxy-2,4-dimethyl-6H-dipyrido[3,2-b:2',3'-e] [1,4]diazepine (0.3 g, 0.75 mmol), methoxylamine hydrochloride (0.15 g, 1.8 mmol) and diisopropylethylamine (0.3 g, 2 mmol) in methylene chloride was stirred at room temperature for 4 days. The organic phase was washed with water, dried, and filtered. The solution was concentrated in vacuo and the residue was chromatographed over silica with 20% ethyl acetate/hexane to give 0.07 g of the title compound, m.p. 164°-166° C.

WORKUP

后处理

  1. washThe organic phase was washed with water
  2. customdried
  3. filtrationfiltered
  4. concentrationThe solution was concentrated in vacuo
  5. customthe residue was chromatographed over silica with 20% ethyl acetate/hexane