反应详情

Iron metal powder (50.2 g; 0.897 mole) and 10M-hydrochloric acid (92 ml; 0.92 mole) were added alternatively over 11/2 hr. to a mixture, of the nitro compound (60.6 g; 0.149 mole) from (a), tetrahydrofuran (520 ml) and water (52 ml), heated under reflux. Heating was continued for a further 31/2 hr. after which the mixture was filtered. The filtrate was evaporated to dryness and the residue partitioned between toluene (500 ml) and water (400 ml). The layers were separated and the toluene solution filtered through kieselguhr, dried and evaporated to give a solid. This material was crystallized from methanol (100 ml) to give the product (41 g; 75%) as a white solid, m.p. 64°-66° C.

1. temperatureunder reflux
2. temperatureHeating
3. custom2 hr
4. filtrationafter which the mixture was filtered
5. customThe filtrate was evaporated to dryness
6. customthe residue partitioned between toluene (500 ml) and water (400 ml)
7. customThe layers were separated
8. filtrationthe toluene solution filtered through kieselguhr
9. customdried
10. customevaporated
11. customto give a solid
12. customThis material was crystallized from methanol (100 ml)
13. customto give the product (41 g; 75%) as a white solid, m.p. 64°-66° C.