HRID1292503

反应详情

EQUATION

反应方程式

HRID 1292503 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 in a solvent mixture of 10 ml of ethanol and 10 ml of pyridine under heat for 30 minutes. The solvents were distilled off under reduced pressure, 50 ml of 5% hydrochloric acid was added, and a formed solid was recovered by filtration, washed with water and then dried to give 3.2 g (yield 93%) of 4-methoxyimino-5-methyl-6-bromothiochroman.

WORKUP

后处理

  1. temperatureunder heat for 30 minutes
  2. distillationThe solvents were distilled off under reduced pressure, 50 ml of 5% hydrochloric acid
  3. additionwas added
  4. filtrationa formed solid was recovered by filtration
  5. washwashed with water
  6. customdried