Lawesson's reagent → HCID 86718492, 화합물
반응식
[Br:1][C:2]1[CH:13]=[CH:12][C:5]2[NH:6][C:7](=O)[CH2:8][CH2:9][NH:10][C:4]=2[CH:3]=1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:23])=CC=1>C1COCC1>[Br:1][C:2]1[CH:13]=[CH:12][C:5]2[NH:6][C:7](=[S:23])[CH2:8][CH2:9][NH:10][C:4]=2[CH:3]=1참가 물질
4
실험 절차
A solution of 7-bromo-4,5-dihydro-1H-benzo[b][1,4]diazepin-2(3H)-one (3) (1.5 g, 6.25 mmol) and Lawesson's Reagent (2.5 g, 12.5 mmol) in THF (50 mL) was heated at 80° C. overnight. The mixture was evaporated, water (50 mL) was added and the solution was extracted with ethyl acetate (100 mL), washed with water (50 mL), dried and concentrated to give the residue, which was purified by CombiFlash (PE:EA=5:1) to afford 7-bromo-4,5-dihydro-1H-benzo[b][1,4]diazepine-2(3H)-thione (1.2 g, yield 75%). LRMS (M+H)+: 256 m/z. 1H NMR (300 MHz, CDCl3) δ 3.13-3.17 (t, J=5.4 Hz, 2H), 3.75-3.79 (t, J=5.4 Hz, 2H), 6.77-6.80 (m, 1H), 6.95-6.98 (m, 2H).