反应详情

A stirred mixture of 7-chloro-1,3-dihydro-3-methyl-5-phenyl-2H-1,4-benzodiazepin-2-one (10 g, 0.035 mol) in pyridine (300 ml), treated with P2S5 (8.0 g, 0.036 mmol) was refluxed, under N2, for 2 hours then concentrated in vacuo. To remove the remaining pyridine the residue was combined with toluene twice with concentration after each addition. The remaining material was mixed with cold NaHCO3 and extracted twice with CH2Cl2. At this point a precipitate thought to be undissolved product formed between the two layers. This was filtered and washed with CH2Cl2 and H2O. The NaHCO3 layer was extracted with CH2Cl2 again. The combined CH2Cl2 extracts were washed with brine, dried over Na2SO4, and concentrated in vacuo. The residue was crystallized from EtOAc-Skelly B to give 3.0 g of the subtitled intermediate, mp 250°. The precipitate was also recrystallized from EtOAc-Skelly B to give 3.01 g of additional subtitled intermediate, mp 255°.

1. temperaturewas refluxed, under N2, for 2 hours
2. concentrationthen concentrated in vacuo
3. customTo remove the remaining pyridine the residue
4. concentrationwas combined with toluene twice with concentration
5. additionafter each addition
6. additionThe remaining material was mixed with cold NaHCO3
7. extractionextracted twice with CH2Cl2
8. customformed between the two layers
9. filtrationThis was filtered
10. washwashed with CH2Cl2 and H2O
11. extractionThe NaHCO3 layer was extracted with CH2Cl2 again
12. washThe combined CH2Cl2 extracts were washed with brine
13. dry with materialdried over Na2SO4
14. concentrationconcentrated in vacuo
15. customThe residue was crystallized from EtOAc-Skelly B