HRID452394

反应详情

EQUATION

反应方程式

HRID 452394 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

A mixture of 2-(bromomethyl)-7-(methylsulfonyl)-4H-1,3-benzodioxine (0.50 g, 1.63 mmol), propan-1-amine (2.0 ml, 24.3 mmol), EtOH (3.0 ml) was heated in a micro wave oven at 140° C. for 30 min. The mixture was evaporated to dryness. The residue was chromathographed on a silica column using EtOAc:MeOH (5:1) as eluent, affording the title compound as a light-yellow solid (0.56 g). The product was washed with several portions of ethyl acetate to give a pure white powder as the title compound (0.43 g, 90%). 0.24 g of the title compound was converted into the hydrochloric acid salt and crystallized from EtOH/DEE. M.p. 213° C. MS m/z (rel. intensity, 70 eV) 285 (M+, 1), 123 (10), 77 (15), 72 (bp), 51 (12).

WORKUP

后处理

  1. customThe mixture was evaporated to dryness