HRID1702623

反应详情

EQUATION

反应方程式

HRID 1702623 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5 g. of 3-carbomethoxy-4-hydroxy-2-methyl-2H-[1]benzothieno[2,3-e]-1,2-thiazine 1,1-dioxide and 3 g. of 2-aminopyridine are treated with 150 ml. of a xylene isomer mixture and heated so that the resulting methanol distils off azeotropically. After 6 hours, the mixture is left to cool to room temperature. The cyrstals obtained are filtered off under suction and washed with a xylene mixture. After recrystallization from dimethylformamide and addition of methanol, there is obtained 4-hydroxy-2-methyl-N-(2-pyridyl)-2H-[1]benzothieno[2,3-e]-1,2-thiazine-3-carboxamide 1,1-dioxide in the form of yellow crystals of melting point 222°-224° C.

WORKUP

后处理

  1. customdistils off azeotropically
  2. waitthe mixture is left
  3. customThe cyrstals obtained
  4. filtrationare filtered off under suction
  5. washwashed with a xylene mixture
  6. customAfter recrystallization
  7. additionfrom dimethylformamide and addition of methanol