HRID1754541

反应详情

EQUATION

反应方程式

HRID 1754541 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 0.33 g (1.0 mmol) of tert-butyl 1-(3-methylbut-2-enoyl)-2,3-dihydro-1H-benzo[e][1,4]diazepine-4(5H)-carboxylate of step 1.1 was irradiated with a 150 W mercury lamp in a immersion well reactor with a pyrex filter in 20 mL of acetone until completion of the reaction monitored by liquid chromatography. The solution was concentrated in vacuo and the residue was purified by column chromatography on silica (eluent: 10-30% ethyl acetate in heptane) to yield 202 mg of the title compound as a beige solid.

WORKUP

后处理

  1. filtrationfilter in 20 mL of acetone until completion of the reaction
  2. concentrationThe solution was concentrated in vacuo
  3. customthe residue was purified by column chromatography on silica (eluent: 10-30% ethyl acetate in heptane)