Sodium Methoxide → 1-(3-(azetidine-1-carbonyl)phenyl)-3-cyclopropyl-5-((2-fluoro-4-iodophenyl)amino)-6,8-dimethylpyrido[4,3-d]pyrimidine-2,4,7(1H,3H,6H)-trione
反応式
[N:1]1([C:5]([C:7]2[CH:8]=[C:9]([NH:13][C:14]3[C:23]4[C:22](=[O:24])[N:21]([CH:25]5[CH2:27][CH2:26]5)[C:20](=[O:28])[N:19]([C:29]5[CH:34]=[CH:33][C:32]([I:35])=[CH:31][C:30]=5[F:36])[C:18]=4[N:17]([CH3:37])[C:16](=[O:38])[C:15]=3[CH3:39])[CH:10]=[CH:11][CH:12]=2)=[O:6])[CH2:4][CH2:3][CH2:2]1.C[O-].[Na+]>O1CCCC1>[N:1]1([C:5]([C:7]2[CH:8]=[C:9]([N:13]3[C:14]4=[C:15]([CH3:39])[C:16](=[O:38])[N:17]([CH3:37])[C:18]([NH:19][C:29]5[CH:34]=[CH:33][C:32]([I:35])=[CH:31][C:30]=5[F:36])=[C:23]4[C:22](=[O:24])[N:21]([CH:25]4[CH2:27][CH2:26]4)[C:20]3=[O:28])[CH:10]=[CH:11][CH:12]=2)=[O:6])[CH2:2][CH2:3][CH2:4]1参加物
4
実験手順
5-((3-(azetidine-1-carbonyl)phenyl)amino)-3-cyclopropyl-1-(2-fluoro-4-iodophenyl)-6,8-dimethylpyrido[2,3-d]pyrimidine-2,4,7(1H,3H,8H)-trione (4b) (0.11 g, 0.17 mmol) was taken in tetrahydrofuran (3 ml) at room temperature, sodium methoxide (25% in MeOH, 371 mg, 1.71 mmol) was added and the reaction mixture was stirred at the same temperature for 1 hr under nitrogen atmosphere. The progress of the reaction was monitored by HPLC. After complete consumption of the substrate, the reaction mixture was diluted with HCl (2 mL, 2 N) and concentrated under vacuum. To the residue DCM (20 ml) was added, the organic layer was dried over sodium sulphate and concentrated under vacuum to give the crude compound which was purified by column chromatography to give the title product (0.09 g).