反应详情

温度

10 °C

10 Mmol of 4'-nitro-2-propoxyacetophenone oxime, 10.4 mmol of 2-chloroethyl amine hydrochloride and 1.4 g of powdered potassium hydroxide were added to 25 ml of dimethyl formamide while stirring at 10° C. After stirring for two days at room temperature the dimethyl formamide was evaporated in vacuo, the residue was brought in water and then 2 N hydrochloric acid was added until pH 3. The remaining oxime was removed by means of ether, after which 30 ml of 2 N sodium hydroxide solution were added. Then three extractions with ether were carried out. The collected ether layers were washed twice with a 5% sodium bicarbonate solution and then dried on sodium sulphate. After removing the ether in vacuo the residue was dissolved in absolute ethanol and converted into the little compound by means of alcoholic hydrochloric acid. After recrystallization from alcohol/ether the melting point was 128°-130° C.

1. customwas evaporated in vacuo
2. addition2 N hydrochloric acid was added until pH 3
3. customThe remaining oxime was removed by means of ether
4. additionafter which 30 ml of 2 N sodium hydroxide solution were added
5. extractionThen three extractions with ether
6. washThe collected ether layers were washed twice with a 5% sodium bicarbonate solution
7. customdried on sodium sulphate
8. customAfter removing the ether in vacuo the residue
9. dissolutionwas dissolved in absolute ethanol
10. customAfter recrystallization from alcohol/ether the melting point was 128°-130° C.