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

HRID 464809ノート

反応式

HRID 464809 の反応式
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

参加物

6

反応物 4

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

生成物 1

HCID 201358121-(1-Methyl-3-phenoxypropyl)piperidine収率 75%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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 the solution was separated with 20% aqueous sodium hydroxide solution. After the ether layer was dried with 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 solvent to give 5.46 g of 1-(1-methyl-3-phenoxypropyl)piperidine in a yield of 75%.

後処理

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

出典と根拠

ORDレコード
ord-5fcc18ac3029427fbd0a24db0cd7705f
出典データセット
uspto-grants-1985_10
特許番号
US04549023

反応ノート

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