反応式
[CH3:1][O:2][C:3]1[CH:19]=[CH:18][CH:17]=[CH:16][C:4]=1[C:5]([CH2:14][CH3:15])([OH:13])[C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][CH:7]=1.C(=O)([O-])[O-].[K+].[K+].[OH-].[CH2:27]([N+:31](CCCC)([CH2:36][CH2:37]CC)[CH2:32][CH2:33]CC)[CH2:28][CH2:29]C.Cl.C(N(CC)CCCCl)C>C(C(C)=O)C(C)C>[CH3:1][O:2][C:3]1[CH:19]=[CH:18][CH:17]=[CH:16][C:4]=1[C:5]([CH2:14][CH3:15])([OH:13])[C:6]1[CH:11]=[CH:10][C:9]([O:12][CH2:29][CH2:28][CH2:27][N:31]([CH2:36][CH3:37])[CH2:32][CH3:33])=[CH:8][CH:7]=1参加物
実験手順
12.9 g. of 2-methoxy-4'-hydroxy-α-ethyl-benzhydrol are dissolved in 100 ml. of methyl isobutyl ketone, 23 g. of anhydrous potassium carbonate 0.4 ml. of a 40% tetrabutyl ammoniumhydroxide solution and 10.3 g. of 3-diethylamino-propyl chloride hydrochloride are added, and the solution is heated up to the boiling point. The reaction mixture is boiled for 4 hours, and the solvent is distilled off under reduced pressure. To the residue water is added, and it is extracted with benzene. The benzene phase is washed with a 5% potassium hydroxide solution and subsequently with water. After drying over anhydrous potassium carbonate, benzene is distilled off under reduced pressure, and the residue is fractionated in vacuo to yield 13.2 g. of the title compound, boiling at 200° to 203° C./13.3 Pa.
後処理
- temperaturethe solution is heated up to the boiling point
- distillationthe solvent is distilled off under reduced pressure
- additionTo the residue water is added
- extractionit is extracted with benzene
- washThe benzene phase is washed with a 5% potassium hydroxide solution and subsequently with water
- dry with materialAfter drying over anhydrous potassium carbonate, benzene
- distillationis distilled off under reduced pressure
- customto yield 13.2 g
出典と根拠
- ORDレコード
- ord-e0b56837ae5643779e5db1a46ccc4680
- 出典データセット
- uspto-grants-1986_08
- 特許番号
- US04605672
関連ノート
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