HRID452410

反应详情

EQUATION

反应方程式

HRID 452410 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Preparation according to Example 3. 7-bromo-2-(bromomethyl)-6-fluoro-4H-1,3-benzodioxine (0.60 g, 1.84 mmol), propan-1-amine (1.0 ml, 12.2 mmol) and EtOH (3.0 ml) was Heated at 130° C. for 40 min. Twice purification by flash column chroma-tography (EtOAc) gave the pure title compound (0.23 g, 41%). The amine was converted into the hydrochloric acid salt and crystallized from EtOH/DEE. M.p. 182° C. MS m/z (rel. intensity, 70 eV) 305 (M+, 3), 303 (M+, 3), 205 (8), 203 (8), 96 (6), 95 (10), 72 (bp).

WORKUP

后处理

  1. customPreparation
  2. customTwice purification by flash column chroma-tography (EtOAc)