反応式
[Cl:1][C:2]1[CH:33]=[CH:32][C:5]([CH2:6][NH:7][C:8]([C:10]2[C:11](=[O:31])[N:12]=[C:13]3[CH:20]=[CH:19][C:18]([C:21]#[C:22][CH2:23][O:24]C4CCCCO4)=[CH:17][N:14]3[C:15]=2[OH:16])=[O:9])=[CH:4][CH:3]=1.Cl>C(Cl)Cl.CO>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][NH:7][C:8]([C:10]2[C:11](=[O:31])[N:12]=[C:13]3[CH:20]=[CH:19][C:18]([C:21]#[C:22][CH2:23][OH:24])=[CH:17][N:14]3[C:15]=2[OH:16])=[O:9])=[CH:32][CH:33]=1参加物
5
実験手順
N-(4-Chlorobenzyl)-4-hydroxy-2-oxo-7-(3-(tetrahydro-2H-pyran-2-yloxy)-1-propynyl)-2H-pyrido[1,2-a]pyrimidine-3-carboxamide (Preparation 7, 12 mg) is dissolved in CH2Cl2 and treated with 0.5 M HCl in methanol (0.5 mL). The reaction mixture is stirred for 16 h at room temperature. The mixture is concentrated, and the residue is crystallized from ether/hexanes and dried to afford 7 mg of the title compound as a brown solid. Physical characteristics: 1H NMR (CD3OD) δ9.2, 8.35, 7.75, 7.4-7.5, 4.80, 4.50; MS (ESI+) m/z 386 (M+H)+.
後処理
- concentrationThe mixture is concentrated
- customthe residue is crystallized from ether/hexanes
- customdried
出典と根拠
- ORDレコード
- ord-e2ddaf5c2a2842ea8b4cb3639a77cc68
- 出典データセット
- uspto-grants-2005_06
- 特許番号
- US06903097B2
関連ノート
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