反应详情

A solution of 3'-acetyl-1-benzyl-2'-hydroxy-1H-tetrazole-5-carboxanilide (2.6 g) in glacial acetic acid (100 ml) was hydrogenated at 52° C. and 4.1 kg/cm2 for 6 hours, using a catalyst of palladium on charcoal (5% w/w). The mixture was filtered and the filtrate was evaporated in vacuo to give a solid residue, which was recrystallised by dissolving in hot dimethylformamide (7 ml) and slowly adding a large volume of water (100 ml). The colourless solid which crystallised out was collected and discarded as an unwanted by-product. The mother liquor was evaporated under diminished pressure, and the resulting residue was recrystallised from a small volume of aqueous dimethylformamide to give 3'-ethyl-2'-hydroxytetrazole-5-carboxanilide (0.3 g) in the form of pale cream crystals, m.p. 185°-187° C.

1. customwas hydrogenated at 52° C.
2. filtrationThe mixture was filtered
3. customthe filtrate was evaporated in vacuo
4. customto give a solid residue, which
5. customwas recrystallised
6. dissolutionby dissolving in hot dimethylformamide (7 ml)
7. additionslowly adding a large volume of water (100 ml)
8. customThe colourless solid which crystallised out
9. customwas collected
10. customThe mother liquor was evaporated under diminished pressure
11. customthe resulting residue was recrystallised from a small volume of aqueous dimethylformamide