Potassium Carbonate → 2-Methoxy-4'-[3-(diethylamino)-propoxy]-alpha-ethyl-benzhydrol

HRID 364651ノート

反応式

HRID 364651 の反応式
[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

6

反応物 4

HCID 11430Potassium CarbonateHCID 145749Diethylaminopropyl chloride, hydrochlorideHCID 2723671Tetrabutylammonium HydroxideHCID 14727321HCID 14727321、化合物

生成物 1

HCID 202395732-Methoxy-4'-[3-(diethylamino)-propoxy]-alpha-ethyl-benzhydrol

試薬・触媒・溶媒 1

HCID 7909Methyl Isobutyl Ketone溶媒

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

  1. temperaturethe solution is heated up to the boiling point
  2. distillationthe solvent is distilled off under reduced pressure
  3. additionTo the residue water is added
  4. extractionit is extracted with benzene
  5. washThe benzene phase is washed with a 5% potassium hydroxide solution and subsequently with water
  6. dry with materialAfter drying over anhydrous potassium carbonate, benzene
  7. distillationis distilled off under reduced pressure
  8. 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

反応ノート

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