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

HRID 3807

반응식

HRID 3807 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-077a49be5a59401b8abfc287ca092333
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04722926

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