Ethanol → Ethyl [2-(4-Benzhydrylpiperidino)-2-oxoethoxy]acetate

HRID 1395480

反応式

HRID 1395480 の反応式
[CH2:1](O)[CH3:2].[CH:4]([CH:17]1[CH2:22][CH2:21][N:20]([C:23](=[O:30])[CH2:24][O:25][CH2:26][C:27]([OH:29])=[O:28])[CH2:19][CH2:18]1)([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.C1(C)C=CC(S(O)(=O)=O)=CC=1>ClCCl>[CH:4]([CH:17]1[CH2:18][CH2:19][N:20]([C:23](=[O:30])[CH2:24][O:25][CH2:26][C:27]([O:29][CH2:1][CH3:2])=[O:28])[CH2:21][CH2:22]1)([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

参加物

5

反応物 3

HCID 702EthanolHCID 6101p-Toluenesulfonic acidHCID 196442Mcn 4308

生成物 1

HCID 54306890Ethyl [2-(4-Benzhydrylpiperidino)-2-oxoethoxy]acetate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To about 50 milliliters of ethanol is added 3.63 grams (10 millimoles) of [2-(4-benzhydrylpiperidino)-2-oxoethoxy]acetic acid (prepared as described in Example V) and 200 milligrams of p-toluenesulfonic acid and the mixture refluxed for about four hours whereupon a reaction takes place with the formation in the reaction mixture of the desired ester product as confirmed by chromatographic analysis. The reaction mixture is subjected to reduced pressure to evaporate the ethanol and to obtain a product residue which is then dissolved in dichloromethane. The dichloromethane solution is first washed with aqueous bicarbonate solution, then dried over potassium carbonate and finally evaporated under reduced pressure to recover an ethyl [2-(4-benzhydrylpiperidino)-2-oxoethoxy]acetate product as residue. The ester product which may be further purified by distillation under reduced pressure has a molecular weight of 391.5.

後処理

  1. temperaturethe mixture refluxed for about four hours whereupon a reaction
  2. customto evaporate the ethanol
  3. customto obtain a product residue which
  4. washThe dichloromethane solution is first washed with aqueous bicarbonate solution
  5. dry with materialdried over potassium carbonate
  6. customfinally evaporated under reduced pressure
  7. customto recover an ethyl [2-(4-benzhydrylpiperidino)-2-oxoethoxy]acetate product as residue
  8. distillationThe ester product which may be further purified by distillation under reduced pressure

出典と根拠

ORDレコード
ord-21f2aca31b5e42c99d20d0b0d8dcbca7
出典データセット
uspto-grants-1980_05
特許番号
US04203991

関連ノート

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