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
4,5-Dihydro-8-methylthio-2-phenylbenzo[2,1-c:3,4-b′]dithiophene-6-carboxylic acid (0.50 g) was dissolved in tetrahydrofuran (10 ml); oxazolyl chloride (0.15 ml) and then N,N-dimethylformamide (one drop) were added. After the mixture was stirred at room temperature for 2 hours, it was concentrated under reduced pressure. The residue was dissolved in tetrahydrofuran (30 ml); concentrated aqueous ammonia (5 ml) was added. After the reaction mixture was stirred at room temperature for one hour, it was poured over water and extracted with chloroform-methanol the organic layer was washed with water and dried (MgSO4), after which the solvent was distilled off to yield 4,5-dihydro-8-methylthio-2-phenylbenzo[2,1-c:3,4-b′]dithiophene-6-carboxamide (0.28 g, 56%), which was recrystallized from ethanol. Melting point 192-193° C.
WORKUP
后处理
- concentrationit was concentrated under reduced pressure
- dissolutionThe residue was dissolved in tetrahydrofuran (30 ml)
- additionconcentrated aqueous ammonia (5 ml) was added
- stirringAfter the reaction mixture was stirred at room temperature for one hour
- additionit was poured over water
- extractionextracted with chloroform-methanol the organic layer
- washwas washed with water
- dry with materialdried (MgSO4)
- distillationafter which the solvent was distilled off