反応式
[I:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([O:8][CH3:9])[C:3]=1[CH:10]=[N:11][C:12]1[C:13]([NH2:25])=[N:14][C:15]([N:19]2[CH2:24][CH2:23][O:22][CH2:21][CH2:20]2)=[N:16][C:17]=1[CH3:18].C1COCC1.C(O)(=O)C.C(O)(=O)C.IC1C=CC=CC=1>CO>[I:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([O:8][CH3:9])[C:3]=1[C:10]1[NH:25][C:13]2[C:12]([N:11]=1)=[C:17]([CH3:18])[N:16]=[C:15]([N:19]1[CH2:20][CH2:21][O:22][CH2:23][CH2:24]1)[N:14]=2参加物
5
実験手順
To a solution of N5-(4-Iodo-2-methoxy-pyridin-3ylmethylene)-6-methyl-2-morpholin-4-yl-pyrimidine-4,5-diamine (140 mg, 0.31 mmol) in a mixture of MeOH:THF (20 mL: 10 mL) was added iodobenzene diacetate (198 mg, 0.62 mmol). After stirring at ambient temperature for 4 hours, the solvents were evaporated in vacuo and the crude was purified by preparative HPLC (see method below) to give the title compound as an amber solid (50 mg, 36%): IR (KBr, cm−1) 3420, 2853, 1618; 1H NMR (400 MHz, CDCl3) δ 9.63 (s, 1H), 7.83 and 7.54 (d, J=5.3, 1H), 3.91 (s, 3H), 3.81–3.77 (m, 8H), 2.72 (s, 3H); LCMS (+ESI, M+H+) m/z 453; HPLC: 97% (220 nm).
後処理
- customthe solvents were evaporated in vacuo
- customthe crude was purified by preparative HPLC (see method below)
出典と根拠
- ORDレコード
- ord-3f6a966281734c0e8afd9d502cafa527
- 出典データセット
- uspto-grants-2007_03
- 特許番号
- US07189716B2
関連ノート
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