HRID1657399

反应详情

EQUATION

反应方程式

HRID 1657399 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

To a suspension of 90 grams (0.352 moles) of methyl 4-hydroxy-2H-1,2-benzothiazine-3-carboxylate 1,1-dioxide in 450 ml proprietory alcohol there is added a solution of 15.5 grams (0.3875 moles) of sodium hydroxide in 450 ml of water at a temperature of less than 20°C. 53.4 Grams (0.423 moles) of dimethyl sulphate is added while stirring, at 25°C. and the mixture is then allowed to stir for about 15 hours. It is cooled to 10°C. and filtered. The cake is washed with water, followed by a 50% alcohol/water wash, and dried. Yield is 90 grams (95%) m.p. 162.5°-164°C.

WORKUP

后处理

  1. stirringto stir for about 15 hours
  2. temperatureIt is cooled to 10°C.
  3. filtrationfiltered
  4. washThe cake is washed with water
  5. washwash
  6. customdried