Diisobutylaluminum hydride → 7-Hydroxymethyl-4-(4-phenoxy-phenylamino)-pyrrolo[1,2-b]pyridazine-3-carbonitrile
반응식
C([O:3][C:4]([C:6]1[N:10]2[N:11]=[CH:12][C:13]([C:29]#[N:30])=[C:14]([NH:15][C:16]3[CH:21]=[CH:20][C:19]([O:22][C:23]4[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=4)=[CH:18][CH:17]=3)[C:9]2=[CH:8][CH:7]=1)=O)C.CC(C[AlH]CC(C)C)C>C1COCC1>[OH:3][CH2:4][C:6]1[N:10]2[N:11]=[CH:12][C:13]([C:29]#[N:30])=[C:14]([NH:15][C:16]3[CH:21]=[CH:20][C:19]([O:22][C:23]4[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=4)=[CH:18][CH:17]=3)[C:9]2=[CH:8][CH:7]=1참가 물질
4
실험 절차
To a solution of 406 (39.8 mg, 0.1 mmol) in THF (2 ml) was added DIBAL-H (1.0 M in CH2Cl2, 0.2 ml, 0.2 mmol) at −78° C. The reaction mixture was stirred at this temperature for 6 h, then at 0° C. for 2 h, quenched with water (0.1 ml). The solid was filtered off, and the filtrate was concentrated. The residue was purified by preparative TLC to give the title compound (22.8 mg, 64%) as a brown solid (2.5% MeOH—CH2Cl2). LCMS Found: (M+H)+=357.