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
In 20 ml of methanol, 1.79 g of 2-(2-phthalimidoethyl)-8H-indeno[1,2-d]thiazole was dissolved. Then, 40 ml of a 40% solution of methylamine in methanol was added, followed by stirring at room temperature for 14 hours. The solvent was then evaporated, and chloroform and 1N hydrochloric acid were added to the resulting residue. The aqueous layer was separated and then neutralized with a 1N aqueous solution of sodium hydroxide, followed by extraction with chloroform. The chloroform layer separated was washed successively with water and a saturated aqueous solution of sodium chloride, followed by drying over anhydrous sodium sulfate. The residue obtained by evaporation of the solvent was dissolved in methanol, and fumaric acid was added thereto. The crystals formed were collected by filtration and then washed successively with methanol and diethyl ether, followed by recrystallization from methanol, whereby 572 mg of 2-(2-aminoethyl)-8H-indeno[1,2-d]thiazole fumarate was obtained.
WORKUP
后处理
- customThe solvent was then evaporated
- additionchloroform and 1N hydrochloric acid were added to the resulting residue
- customThe aqueous layer was separated
- extractionfollowed by extraction with chloroform
- customThe chloroform layer separated
- washwas washed successively with water
- dry with materialby drying over anhydrous sodium sulfate
- customThe residue obtained by evaporation of the solvent
- customThe crystals formed
- filtrationwere collected by filtration
- washwashed successively with methanol and diethyl ether
- customfollowed by recrystallization from methanol