HRID1927695

反应详情

EQUATION

反应方程式

HRID 1927695 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

8.9 kg of 5-bromo-2,4-dihydroxybenzoic acid are dissolved in 70 l of methanol and heated to 55° C. 800 ml of sulfuric acid (w=95-98%) are subsequently metered in, and the mixture is stirred under gentle reflux for 4 days, during which a further 500 ml of sulfuric acid (w=95-98%) were added daily (3 times). The reaction mixture is stirred into a cooled solution (5° C.) of 9 kg of sodium hydrogencarbonate in 100 l of water. Filtration and drying in vacuo at 50° C. gives 7.87 kg (83%) of methyl 5-bromo-2,4-dihydroxybenzoate (white crystals), MW 247.1.

WORKUP

后处理

  1. additionwere added daily (3 times)
  2. filtrationFiltration
  3. customdrying in vacuo at 50° C.