HRID840186
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 2-bromo-4-chloro-phenol (99.24 g, 480 mmol) in acetic acid (110 ml) and acetic anhydride (125 ml) was cooled to −10EC. Within 1 hour a solution containing 100% nitric acid (33 ml) and acetic acid (40 ml) was added between −10E and −5EC, with stirring. The mixture was stirred for an additional 1.5 hours at 0-5EC, then the suspension poured onto 300 g of ice in 700 ml of water and stirred for a further 0.5 hour. The solid was collected, washed, and dried to give 97.12 g (80.1%) of the title compound (mp 121-2EC).
WORKUP
后处理
- additionwas added between −10E and −5EC,
- stirringThe mixture was stirred for an additional 1.5 hours at 0-5EC
- stirringstirred for a further 0.5 hour
- customThe solid was collected
- washwashed
- customdried