HRID577577

反应详情

EQUATION

反应方程式

HRID 577577 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 7-bromo-4-(4-methoxybenzyl)-6-methyl-3,4-dihydro-1,4-benzoxazepin-5(2H)-one (130c, 2.8 g, 7.4 mmol) in TFA (30 mL) was refluxed for 14 hours. The reaction mixture was concentrated under vacuum. The residue was purified by column chromatography (petroleum ether/EtOAc, 3/1) to give 7-bromo-6-methyl-3,4-dihydro-1,4-benzoxazepin-5(2H)-one (7-bromo-6-methyl-3,4-dihydro-1,4-benzoxazepin-5(2H)-one (130d, 1.2 g, 63%) as a brown solid.

WORKUP

后处理

  1. temperaturewas refluxed for 14 hours
  2. concentrationThe reaction mixture was concentrated under vacuum
  3. customThe residue was purified by column chromatography (petroleum ether/EtOAc, 3/1)