HRID1762975

反应详情

EQUATION

反应方程式

HRID 1762975 的结构方程式

PROCEDURE

实验过程

According to the U.S. Pat. No. 4,496,737 (Merck) 3-(methylthio)-propionitrile was used as a starting material, which was converted into the corresponding imino-ether base with a yield of 67.2%. The oily product obtained was boiled with 1.5 molar equivalents of sulfamide, for 20 hours. After recovering the excess of sulfamide the product was isolated by column chromatography, with a moderate (26.0%) yield. The N-sulfamyl-3-(methylthio)-propionamide obtained was oxidized into the corresponding sulfoxide with m-chloroperbenzoic acid in a mixture of chloroform and methanol (yield: 83.4%). The sulfoxide compound was then subjected to an elimination reaction by boiling with triethyl amine in an ethanolic medium for 20 to 30 hours. As a result, N-sulfamyl-acrylic amidine of the formula (IV) ##STR6## was isolated by column chromatography with a yield of 37.2%.

WORKUP

后处理

  1. customThe oily product obtained
  2. customAfter recovering the excess of sulfamide the product
  3. customwas isolated by column chromatography, with a moderate (26.0%)
  4. customyield