反应详情

3.0 g of ammonium chloride and 50 g of zinc powder are added to 150 ml of an aqueous-alcoholic solution (85% of alcohol and 15% of water). This mixture is heated to the reflux temperature, whilst stirring, and 0.1 mol (25.7 g) of 2-chloro-4-nitro-N-tetrahydrofurfurylaniline is then added gradually. When the addition has ended and the reaction mixture is decolorised, the latter is filtered and the filtrate is collected in 20 ml of ice-cooled hydrochloric acid. After cooling, the expected hydrochloride precipitates in the form of crystals. It is filtered off, washed with a small amount of ice-cooled absolute alcohol and dried in vacuo. It melts at about 170° C. with decomposition.

1. temperatureThis mixture is heated to the reflux temperature
2. additionWhen the addition
3. filtrationthe latter is filtered
4. customthe filtrate is collected in 20 ml of ice-
5. temperaturecooled hydrochloric acid
6. temperatureAfter cooling
7. customthe expected hydrochloride precipitates in the form of crystals
8. filtrationIt is filtered off
9. washwashed with a small amount of ice-
10. temperaturecooled absolute alcohol
11. customdried in vacuo