반응 #1572581

반응 방정식

1-benzyl-1H-benzo[b][1,4]diazepine-2,4(3H,5H)-dione

P2S5

→

1-benzyl-4-thioxo-4,5-dihydro-1H-benzo[b][1,4]diazepin-2(3H)-one

수율 30.0%

용매

pyridine

반응 조건

후처리

1. 1
   온도to reflux
2. 2
   기타The solvent was evaporated in vacuo
3. 3
   기타the residue was purified by prep-TLC (DCM:MeOH=50:1)

실험 절차

A solution of 1-benzyl-1H-benzo[b][1,4]diazepine-2,4(3H,5H)-dione (160 mg, 0.60 mmol) and P2S5 (140 mg, 0.63 mmol) in 20 mL of pyridine was heated to reflux and stirred for 1 h under N2 atmosphere. The solvent was evaporated in vacuo, the residue was purified by prep-TLC (DCM:MeOH=50:1) to give 1-benzyl-4-thioxo-4,5-dihydro-1H-benzo[b][1,4]diazepin-2(3H)-one (50 mg, 30%). 1H NMR (300 MHz, DMSO): δ 3.74 (q, J=12.3 Hz, J=12.3 Hz, 1H), 5.12 (q, J=15.6 Hz, J=15.9 Hz, 1H), 7.03-7.06 (m, 2H), 7.17-7.27 (m, 6H), 7.48 (d, J=7.5 Hz, 1H).

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