HCID 20186023、化合物 → HCID 20186009、化合物
反応式
[N:1]1([CH2:7][C:8]2[CH:9]=[C:10]([CH:30]=[CH:31][CH:32]=2)[O:11][CH2:12][CH2:13][CH2:14][C:15]2[NH:20][C:19](=[O:21])[C:18]([O:22]CC3C=CC=CC=3)=[CH:17][N:16]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1>Cl>[N:1]1([CH2:7][C:8]2[CH:9]=[C:10]([CH:30]=[CH:31][CH:32]=2)[O:11][CH2:12][CH2:13][CH2:14][C:15]2[NH:20][C:19](=[O:21])[C:18]([OH:22])=[CH:17][N:16]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1参加物
実験手順
2-[3-[3-(Piperidinomethyl)phenoxy]propyl]-5-benzyloxypyrimidin-4-one (0.68 g) was stirred under reduced pressure and taken to pH 8 with hours in lN hydrochloric acid (20 ml). The mixture was concentrated under reduced pressure and taken to pH 8 with aqueous sodium bicarbonate. This mixture was extracted with n-butanol (3×20 ml); these extracts were combined, washed with water (2'5 ml), dried (MgSO4) and evaporated under reduced pressure to give the title compound. This was dissolved in methanol containing ethanolic HCl, excess solvent was evaporated under reduced pressure and the residue crystallised from isopropanol-acetone to give 2-[3-[3-(piperidinomethyl)phenoxy]propyl]-5-hydroxypyrimidin -4-one dihydrochloride (0.24 g), m.p. 192°-4° C.
後処理
- concentrationThe mixture was concentrated under reduced pressure
- extractionThis mixture was extracted with n-butanol (3×20 ml)
- washwashed with water (2'5 ml),
- dry with materialdried (MgSO4)
- customevaporated under reduced pressure
出典と根拠
- ORDレコード
- ord-24b85461beab4b6a9fbd6be26f0676f3
- 出典データセット
- uspto-grants-1987_09
- 特許番号
- US04694008
反応ノート
読み込み中…