HRID1447163

反应详情

EQUATION

反应方程式

HRID 1447163 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

95 parts of isopropylaminosulfonyl chloride were stirred into a mixture of 96 parts of N-carbomethoxy-O-isopropylisourea and 73 parts of triethylamine in 700 parts of tetrahydrofuran in the course of 25 minutes, at 10°-15° C. After having been stirred for one hour at 25° C., the reaction mixture was extracted once with water and once with 0.5 N hydrochloric acid, dried and concentrated under reduced pressure. This gave 130 parts of N-carbomethoxy-N'-isopropylsulfamyl-O-isopropylisourea, of melting point 62°-64° C. 33.7 parts of this product were cyclized by means of 17.6 parts of 50% strength by weight sodium hydroxide solution in 30 parts of water in the course of 5 minutes at from 55° to 60° C. Extraction with ether, acidification, washing with water and drying gave 22 parts of 6-isopropyl-3-isopropoxy-5,6-dihydro-1,2,4,6-thiatriazin-5-one-1,1-dioxide, of melting point 164°-167° C. This constitutes active ingredient No. 4.

WORKUP

后处理

  1. extractionthe reaction mixture was extracted once with water and once with 0.5 N hydrochloric acid
  2. customdried
  3. concentrationconcentrated under reduced pressure