反应详情

The acid from (b) (2.0 g) was added to a mixture of concentrated sulphuric acid (15 ml) and 1,2-dichloroethane (10 ml) kept at 0°. Potassium nitrate (1.2 g) was then added in portions with stirring over a period of 30 minutes, keeping the temperature at 0°. The mixture was stirred for a further hour at 0° and then for 3 hours at room temperature. The mixture was then poured on to ice and extracted with ethyl acetate. The extract was washed with water, dried, and evaporated to give a dark gum. This was extracted several times with boiling cyclohexane. The residue crystallised on cooling and was identified as the required nitro-acid, with a melting point of 147°-148°.

1. customkept at 0°
2. customat 0°
3. stirringThe mixture was stirred for a further hour at 0°
4. waitfor 3 hours at room temperature
5. additionThe mixture was then poured on to ice
6. extractionextracted with ethyl acetate
7. washThe extract was washed with water
8. customdried
9. customevaporated
10. customto give a dark gum
11. extractionThis was extracted several times with boiling cyclohexane
12. customThe residue crystallised
13. temperatureon cooling