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

HRID 1395480

반응식

HRID 1395480 반응식
[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

참가 물질

5

반응물 3

HCID 702EthanolHCID 6101p-Toluenesulfonic acidHCID 196442Mcn 4308

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-21f2aca31b5e42c99d20d0b0d8dcbca7
출처 데이터셋
uspto-grants-1980_05
특허 번호
US04203991

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