Diethyl Ether → 1-(1-Methyl-3-phenoxypropyl)piperidine

HRID 484831노트

반응식

HRID 484831 반응식
S(C1C=CC(C)=CC=1)(O[CH:5]([CH2:7][CH2:8][O:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[CH3:6])(=O)=O.[NH:23]1[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]1.C(OCC)C.C(Cl)(Cl)Cl>CO>[CH3:6][CH:5]([N:23]1[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]1)[CH2:7][CH2:8][O:9][C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 6212ChloroformHCID 8082PiperidineHCID 133267624-Phenoxy-2-butyl tosylate

생성물 1

HCID 201358121-(1-Methyl-3-phenoxypropyl)piperidine수율 75%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

In a sealed tube, 10 g of the 4-phenoxy-2-butyl tosylate was reacted with 11.2 g of piperidine in 60 ml of absolute methyl alcohol for one hour at 125° C. After the reaction solution was condensed under reduced pressure, 100 ml of diethyl ether was added into the solution, and then the solution was separated into the diethyl ether solution and 20% aqueous sodium hydroxide solution. After the ether layer was dried over anhydrous sodium sulfate, ether was removed under reduced pressure therefrom. The residue thus obtained was subjected to an alumina-column chromatography using chloroform as the developing solvent to give 5.46 g of 1-(1-methyl-3-phenoxypropyl)piperidine in a yield of 75%.

후처리

  1. additionwas added into the solution
  2. customthe solution was separated into the diethyl ether solution and 20% aqueous sodium hydroxide solution
  3. dry with materialAfter the ether layer was dried over anhydrous sodium sulfate, ether
  4. customwas removed under reduced pressure
  5. customThe residue thus obtained

출처 및 근거

ORD 기록
ord-60be75fe60f94abda7ab5e3317ecab52
출처 데이터셋
uspto-grants-1985_08
특허 번호
US04533731

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