HRID1834878

反应详情

EQUATION

反应方程式

HRID 1834878 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 12 g. of 1-ethoxycarbonylmethylthio-2-nitro-2-methylpropionaldoxime and 150 ml of ammonium hydroxide was charged into a pyrex pressure bottle and stirred at room temperature for three days. The excess ammonia and water was stripped from the reaction mixture under reduced pressure. The solid crystalline residue was washed with a small amount of cold water and dried. The residue was then recrystallized from acetonitrile to yield 4 g of 2-Oximino-3,3-dimethyltetrahydro-1,4-thiazin-5-one, m.p. 234°-236° C. The nmr and infrared spectra supported the proposed structure.

WORKUP

后处理

  1. additionA mixture of 12 g
  2. washThe solid crystalline residue was washed with a small amount of cold water
  3. customdried
  4. customThe residue was then recrystallized from acetonitrile