Water → 1-Ethyl-2-(4-chlorobenzyl)perhydroazepine

HRID 27429

反応式

HRID 27429 の反応式
[Cl:1][C:2]1[CH:15]=[CH:14][C:5]([CH2:6][CH:7]2[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][NH:8]2)=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:22](Br)[CH3:23].O>C(C(C)=O)C>[CH2:22]([N:8]1[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH:7]1[CH2:6][C:5]1[CH:14]=[CH:15][C:2]([Cl:1])=[CH:3][CH:4]=1)[CH3:23]

参加物

6

反応物 4

HCID 962WaterHCID 6332Ethyl BromideHCID 11430Potassium CarbonateHCID 39338092-[(4-Chlorophenyl)methyl]azepane

生成物 1

HCID 233428031-Ethyl-2-(4-chlorobenzyl)perhydroazepine

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

Boil together (under agitation) 4 g of 2-(4-chlorobenzyl)perhydroazepine, 2.5 g of anhydrous potassium carbonate and 2.9 g of ethyl bromide under reflux for 26 hours in 30 ml of ethylmethylketone. Cool the thus-produced reaction mixture to ambient temperature. Mix the cooled reaction mixture with water and then extract it with diethyl ether. Dry the resulting organic phase over sodium sulfate, remove the ether and distil the residue to obtain 5.12 g (70% of theory) of the title compound with a BP of 112° at 0.005 mm of Hg.

後処理

  1. temperatureCool
  2. customthe thus-produced reaction mixture to ambient temperature
  3. additionMix
  4. extractionextract it with diethyl ether
  5. dry with materialDry the resulting organic phase over sodium sulfate
  6. customremove the ether
  7. customdistil the residue

出典と根拠

ORDレコード
ord-61b6237faed14f6ea997de5e8a8ecfe3
出典データセット
uspto-grants-1980_09
特許番号
US04221788

関連ノート

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