HRID1447120

反应详情

EQUATION

反应方程式

HRID 1447120 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2.5 g powdered potassium hydroxide, 0.1 g. of dicyclohexyl-18-crown-6, and 6.0 g (0.037 mole) of 1-methylthio-3,3-dimethyl-2-butanone oxime in 200 ml of benzene was stirred 2 hrs. at 28° C. Then 5.9 g (0.037 mole) of N-methyl-N-(dimethylaminosulfenyl)carbamoyl fluoride was added rapidly. The mixture was stirred 20 hrs. at room temperature, water washed three times, dried (MgSO4), and the benzene solvent was removed in vacuo. The product, 1-methylthio-3,3-dimethyl-2-butanone O-[N-methyl-N-(dimethylaminosulfenyl)carbamoyl]oxime, was obtained as a heavy syrup which would not crystallize, 8 g. (73.7 percent yield).

WORKUP

后处理

  1. additionA mixture of 2.5 g
  2. customat 28° C
  3. washat room temperature, water washed three times
  4. dry with materialdried (MgSO4)
  5. customthe benzene solvent was removed in vacuo