HRID1720226

反应详情

EQUATION

反应方程式

HRID 1720226 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureunder heat in a mixed solvent
  2. distillationThe solvents were distilled off under reduced pressure
  3. addition50 ml of 5% hydrochloric acid was added
  4. customto form a solid
  5. filtrationThe solid was recovered by filtration
  6. washwashed with water
  7. customdried