Lawesson's reagent → (11aS)-1,2,3,10,11,11a-Hexahydro-5H-Pyrrolo[2,1-c][1,4]Benzodiazepin-5-Thione
反応式
[CH2:1]1[C@H:5]2[CH2:6][NH:7][C:8]3[CH:15]=[CH:14][CH:13]=[CH:12][C:9]=3[C:10](=O)[N:4]2[CH2:3][CH2:2]1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:25])=CC=1>C1(C)C=CC=CC=1>[CH2:1]1[C@H:5]2[CH2:6][NH:7][C:8]3[CH:15]=[CH:14][CH:13]=[CH:12][C:9]=3[C:10](=[S:25])[N:4]2[CH2:3][CH2:2]1参加物
4
実験手順
To 50 ml of toluene, there were added 2.02 g of (11aS)-1,2,3,10,11,11a-hexahydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-5-one prepared in Reference Example 24 and 4.04 g of the Lawesson's reagent and the mixture was heated under reflux for one hour. After cooling the reaction solution, it was concentrated. The resulting residue was subjected to silica gel column chromatography and then eluted with chloroform/acetone (99/1). The elute was concentrated and recrystallized from ethyl acetate to give 1.6 g (yield 73.3%) of the title compound.