HRID1680636
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
9.7 g. (0.026 moles) of 3-hydroxy-2-phenyl-5,6,7,8-tetrahydrothiazolo[2,3-b]benzothiazolium bromide, prepared according to Example 10, is suspended in a mixture of 1000 ml. methylene chloride and 500 ml. water, and the mixture is stirred at room temperature for 5 hours. The layers are separated and the methylene chloride layer is dried over anhydrous magnesium sulfate. The drying agent is removed by filtration and the filtrate is reduced in volume. The residual solid is triturated with ether and the yellow solid is collected. The crude material is recrystallized from 1.5 l. of acetonitrile to yield a yellow solid weighing 4.7 g. (63% yield). The product melts at ca. 200° C.(dec.).
WORKUP
后处理
- additionis suspended in a mixture of 1000 ml
- customThe layers are separated
- dry with materialthe methylene chloride layer is dried over anhydrous magnesium sulfate
- customThe drying agent is removed by filtration
- customThe residual solid is triturated with ether
- customthe yellow solid is collected
- customThe crude material is recrystallized from 1.5 l
- customof acetonitrile to yield a yellow solid