反应详情

温度

50 °C

Solution of 12.3 g of 3-diethylamino-8-methyl-3,4-dihydrocarbostyril hydrochloride in 100 ml of anhydrous dimethylformamide was added 1.9 g of 60%-sodium hydride, then this mixture was heated at 50° C. for 30 minutes. Next, to this reaction mixture was added dropwise 6.53 g of methyl iodide under ice-cooling condition. After the dropwise addition, the whole mixture was heated at 50° to 60° C. with stirring. The reaction mixture was poured in water, and was extracted with chloroform. The chloroform layer was washed with water, and dried. Chloroform was removed by evaporation, and the residue thus obtained was converted into a hydrochloride, and recrystallized from acetone-n-hexane to obtain 12 g of 1-methyl-3-diethylamino-8-methyl-3,4-dihydrocarbostyril hydrochloride. Light brown powdery substance. Melting point: 162.5°-164.5° C.

1. temperaturecooling condition
2. additionAfter the dropwise addition
3. temperaturethe whole mixture was heated at 50° to 60° C.
4. extractionwas extracted with chloroform
5. washThe chloroform layer was washed with water
6. customdried
7. customChloroform was removed by evaporation
8. customthe residue thus obtained
9. customrecrystallized from acetone-n-hexane