HRID1702623
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customdistils off azeotropically
- waitthe mixture is left
- customThe cyrstals obtained
- filtrationare filtered off under suction
- washwashed with a xylene mixture
- customAfter recrystallization
- additionfrom dimethylformamide and addition of methanol