HRID2306489

反应详情

EQUATION

反应方程式

HRID 2306489 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The fumarate obtained is taken up in methylene chloride/saturated sodium bicarbonate solution and the organic phase is dried and concentrated. 3.09 g of the thus-obtained [4-[6-(allyl-methyl-amino)-hexyloxy]-2-methoxy-phenyl]-(4-bromo-phenyl)-methanone are boiled in 13 ml of acetic acid/7.7 ml of 62% HBr solution at 90° C. for 2 hrs. The reaction mixture is concentrated and the residue is converted into the free base with methylene chloride/saturated sodium bicarbonate solution. The residue is treated with 0.74 g of fumaric acid and processed using ethanol/ether. There are obtained 2.05 g of [4-[6-(allyl-methyl-amino)-hexyloxy]-2-hydroxy-phenyl]-(4-bromo-phenyl)-methanone fumarate, MS: m/e 446 (M+H+, 1Br).

WORKUP

后处理

  1. customthe organic phase is dried
  2. concentrationconcentrated
  3. concentrationThe reaction mixture is concentrated
  4. additionThe residue is treated with 0.74 g of fumaric acid