HRID1447157

反应详情

EQUATION

反应方程式

HRID 1447157 的结构方程式

PROCEDURE

实验过程

154 parts of phosphorus pentachloride were added, in the course of 2 minutes, to a stirred mixture of 128 parts of 6-ethyl-3-methoxy-6H-1,2,4,6-thiatriazin-5-one-1,1-dioxide and 840 parts of phosphorus oxychloride at 25° C. The reaction mixture was then stirred for 51/2 hours under reflux, after which it was evaporated down under reduced pressure. The oil which remained was taken up in 300 parts of 1,2-dichloroethane and the solution was chromatographed over neutral alumina (Activity I). After evaporating down, 127.5 parts (91% of theory) of 5-chloro-6-ethyl-3-methoxy-6H-1,2,4,6-thiatriazine-1,1-dioxide, of melting point 63°-70° C., were obtained (Compound No. 2).

WORKUP

后处理

  1. temperatureunder reflux
  2. customafter which it was evaporated down under reduced pressure
  3. customthe solution was chromatographed over neutral alumina (Activity I)
  4. customAfter evaporating down