Sodium bis(trimethylsilyl)amide → HCID 10077301、化合物

反応式

Cl[C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH2:15][CH2:16][CH2:17][N:18]3[CH2:23][CH2:22][N:21]([CH2:24][CH2:25][F:26])[CH2:20][CH2:19]3)=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[CH:4][N:3]=1.[Cl:27][C:28]1[CH:36]=[C:35]([C:37]#[C:38][CH2:39][CH2:40][O:41][CH3:42])[C:31]2[O:32][CH2:33][O:34][C:30]=2[C:29]=1[NH2:43].C[Si]([N-][Si](C)(C)C)(C)C.[Na+]>CN(C=O)C>[Cl:27][C:28]1[CH:36]=[C:35]([C:37]#[C:38][CH2:39][CH2:40][O:41][CH3:42])[C:31]2[O:32][CH2:33][O:34][C:30]=2[C:29]=1[NH:43][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH2:15][CH2:16][CH2:17][N:18]3[CH2:23][CH2:22][N:21]([CH2:24][CH2:25][F:26])[CH2:20][CH2:19]3)=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[CH:4][N:3]=1

参加物

実験手順

This was prepared by the method described in example 4 using 4-chloro-7-{3-[4-(2-fluoroethyl)piperazin-1-yl]propoxy}-6-methoxyquinazoline (200 mg, 0.52 mmol), 5-chloro-7-(4-methoxybut-1-yn-1-yl)-1,3-benzodioxol-4-amine (146 mg, 0.57 mmol) and sodium bis(trimethylsilyl)amide (1.0M in THF, 1.10 ml) in DMF (3 ml). The crude product was purified by column chromatography on silica using increasing concentrations of methanol in dichloromethane as eluent. There was thus obtained the title compound (187 mg, 60%) as colourless solid, NMR Spectrum:(CDCl3) 2.10 (quintet, 2H), 2.57 (m, 8H), 2.67 & 2.72 (dt, 2H), 2.74 (t, 2H), 3.41 (s, 3H), 3.60 (t, 2H), 3.98 (s, 3H), 4.23 (t, 2H), 4.51 & 4.63 (dt, 2H), 6.06 (s, 2H), 6.85 (s, 1H), 7.04 (s, 1H), 7.08 (s, 1H), 7.28 (s, 1H), 8.61 (s, 1H); Mass Spectrum: M+H+ 600/602