HRID329713
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 mixture of 5.1 g of methyl 6-chloro-3,4-dihydro-2,4-dimethyl-3-oxo-2H-1,4-benzoxazine-8-carboxylate, 20 ml of ethanol and 50 ml of 4% aqueous potassium hydroxide solution is refluxed with heating for 5 hours. The resultant solution is cooled and 350 ml of water is added thereto followed by filtration. The filtrate is made acid with concentrated hydrochloric acid. The precipitated crystals are collected by filtration, washed with water and dried, and then recrystallized from ethanol to give 4.28 g of 6-chloro-3,4-dihydro-2,4-dimethyl-2H-1,4-benzoxazine-8-carboxylic acid, melting at 191°14 193° C.
WORKUP
后处理
- temperatureis refluxed
- temperaturewith heating for 5 hours
- filtrationthereto followed by filtration
- filtrationThe precipitated crystals are collected by filtration
- washwashed with water
- customdried
- customrecrystallized from ethanol