Methanol → HCID 67582065、化合物
反応式
[OH:1][C@@H:2]1[CH2:6][O:5][CH2:4][C@H:3]1[O:7][C:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[N:11]=[C:10]([N:18]2[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]2)[N:9]=1.C[OH:25]>>[C:6]([OH:25])(=[O:5])[CH3:2].[OH:1][C@@H:2]1[CH2:6][O:5][CH2:4][C@H:3]1[O:7][C:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[N:11]=[C:10]([N:18]2[CH2:19][CH2:20][NH:21][CH2:22][CH2:23]2)[N:9]=1参加物
3
実験手順
4-[(3R,4R)-(4-Hydroxytetrahydrofuran-3-yl)oxy]-2-(1-piperazinyl)quinazoline (cf. Example 19) (758 mg) is dissolved in methanol, and the mixture is evaporated to dryness under reduced pressure. The residue is dissolved in acetone (15 ml), and the mixture is filtered, and to the filtrate is added acetic acid (202 mg), and the mixture is allowed to stand at room temperature. The precipitated crystals are separated by filtration to give 4-[(3R,4R)-(4-hydroxytetrahydrofuran-3-yl)oxy]-2-(1-piperazinyl) quinazoline monoacetate (796 mg) as crystals.
後処理
- customthe mixture is evaporated to dryness under reduced pressure
- dissolutionThe residue is dissolved in acetone (15 ml)
- filtrationthe mixture is filtered
- additionto the filtrate is added acetic acid (202 mg)
- customto stand at room temperature