HRID274421

反应详情

EQUATION

反应方程式

HRID 274421 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.75 g of 2-diethylaminoethyl mercaptan hydrochloride are slowly treated with 3.3 g of a 50% strength sodium hydride in oil suspension in 100 ml of THF under a nitrogen atmosphere. After 1 hour, 5 g of 3-phenyl-4-nitrofuroxan are introduced and the mixture is stirred for 20 hours. The inorganic salts are filtered off with suction and the filtrate is concentrated. The residue is taken up in water and extracted with methylene chloride. After drying and concentrating, the residue is dissolved in ethyl acetate and the product is precipitated by introducing hydrogen chloride and filtered off with suction.

WORKUP

后处理

  1. filtrationThe inorganic salts are filtered off with suction
  2. concentrationthe filtrate is concentrated
  3. extractionextracted with methylene chloride
  4. customAfter drying
  5. concentrationconcentrating
  6. dissolutionthe residue is dissolved in ethyl acetate
  7. customthe product is precipitated
  8. additionby introducing hydrogen chloride
  9. filtrationfiltered off with suction