1-Phenylpiperazine → 1-Phenoxy-4-(4-phenyl-1-piperazinyl)-2-butanol
反応式
[C:1]1([N:7]2[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[CH2:14][CH2:15][CH:16]([OH:25])[CH2:17][O:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.C(=O)([O-])[O-].[Na+].[Na+]>C(O)CCC>[O:18]([CH2:17][CH:16]([OH:25])[CH2:15][CH2:14][N:10]1[CH2:11][CH2:12][N:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[CH2:8][CH2:9]1)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1参加物
5
実験手順
A mixture of 6.5 g (0.04 mole) of 1-phenylpiperazine, 8.4 g (0.042 mole) of 4-chloro-1-phenoxy-2-butanol and 15.9 g (0.15 mole) of anhydrous sodium carbonate in 200 ml of 1-butanol was heated at reflux 20 hr. The mixture was concentrated under reduced pressure and the residue was partitioned between water and benzene. The benzene layer was washed with water and aqueous saturated sodium chloride solution, dried over sodium sulfate and concentrated under reduced pressure to give the title product in the residue which was recrystallized from isopropyl alcohol to give 8.9 g (68%) of white powder, m.p. 93°-94° C.
後処理
- temperaturewas heated
- temperatureat reflux 20 hr
- concentrationThe mixture was concentrated under reduced pressure
- customthe residue was partitioned between water and benzene
- washThe benzene layer was washed with water and aqueous saturated sodium chloride solution
- dry with materialdried over sodium sulfate
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-303220ce004d4fad8b1340743f36b87e
- 出典データセット
- uspto-grants-1989_02
- 特許番号
- US04806555
反応ノート
読み込み中…