反应详情

35 g of the foregoing propionoanilide are heated to reflux in 40 ml of glacial acetic acid and 200 ml of absolute toluene for 15 minutes. The residue obtained after distillation of the solvent is treated with methylene chloride and 10% sodium bicarbonate solution. The methylene chloride solution is washed twice with 10% sodium bicarbonate solution and once with water, dried over sodium sulfate, filtered and concentrated. The residue is taken up in benzene, some racemate formed crystallising out and being filtered off. The benzene solution is evaporated and the residue crystallised from ether to give (+)-5-(o-chlorophenyl)-1,3-dihydro-3-methyl-7-nitro-2H-1,4-benzodiazepin-2-one which melts at 198°-200° C and exhibits a rotation of [α]25D =+252.1° (in methylene chloride, 1%).

1. customThe residue obtained
2. distillationafter distillation of the solvent
3. additionis treated with methylene chloride and 10% sodium bicarbonate solution
4. washThe methylene chloride solution is washed twice with 10% sodium bicarbonate solution and once with water
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated
8. customsome racemate formed
9. customcrystallising out
10. filtrationbeing filtered off
11. customThe benzene solution is evaporated
12. customthe residue crystallised from ether