HRID1720226
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
3.0 Grams (12 mmol) of 5-methyl-6-bromothiochroman-4-one and 1.9 g (23 mmol) of O-methylhydroxylamine hydrochloride were refluxed under heat in a mixed solvent containing 10 ml of ethanol and 10 ml of pyridine for 30 minutes. The solvents were distilled off under reduced pressure, and then 50 ml of 5% hydrochloric acid was added to form a solid. The solid was recovered by filtration, washed with water and dried to give 3.2 g of 4-methoxyimino-5-methyl-6-bromothiochroman (yield 93%).
WORKUP
后处理
- temperatureunder heat in a mixed solvent
- distillationThe solvents were distilled off under reduced pressure
- addition50 ml of 5% hydrochloric acid was added
- customto form a solid
- filtrationThe solid was recovered by filtration
- washwashed with water
- customdried