Dimethyl Sulfoxide → 1-(4-Methylbenzyl)-4-(3-chloropropyl)piperazine dihydrochloride

HRID 3807

反応式

HRID 3807 の反応式
[CH3:1][C:2]1[CH:14]=[CH:13][C:5]([CH2:6][N:7]2[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]2)=[CH:4][CH:3]=1.[OH-].[K+].CS(C)=O.Br[CH2:22][CH2:23][CH2:24][Cl:25]>O>[ClH:25].[ClH:25].[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][N:7]2[CH2:12][CH2:11][N:10]([CH2:22][CH2:23][CH2:24][Cl:25])[CH2:9][CH2:8]2)=[CH:13][CH:14]=1

参加物

6

反応物 4

HCID 679Dimethyl SulfoxideHCID 80061-Bromo-3-chloropropaneHCID 14797Potassium HydroxideHCID 7647231-(4-Methylbenzyl)piperazine

生成物 1

HCID 201531921-(4-Methylbenzyl)-4-(3-chloropropyl)piperazine dihydrochloride収率 274.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 14.0 g of 1-(4-methylbenzyl)piperazine, 8.0 g of potassium hydroxide and 125 ml of dimethyl sulfoxide was stirred for 45 minutes. 11.8 g of 1-bromo-3-chloropropane were then added, and the mixture was stirred for an additional hour. Water was added, and the product was extracted with ether, and the extract was dried (sodium sulfate) and treated with ethereal hydrochloric acid to give 23.3 g (94% of theory) of 1-(4-methylbenzyl)-4-(3-chloropropyl)piperazine dihydrochloride as a white crystalline solid.

後処理

  1. stirringthe mixture was stirred for an additional hour
  2. extractionthe product was extracted with ether
  3. dry with materialthe extract was dried (sodium sulfate)
  4. additiontreated with ethereal hydrochloric acid

出典と根拠

ORDレコード
ord-077a49be5a59401b8abfc287ca092333
出典データセット
uspto-grants-1988_02
特許番号
US04722926

関連ノート

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