Hydrochloric Acid → 1-(3,3-Diphenylpropyl)-4(3,4-dimethoxybenzyl)piperazine dihydrochloride

HRID 1076786노트

반응식

HRID 1076786 반응식
[C:1]1([CH:7]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH2:8][CH2:9][N:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:22][O:23][C:24]1[CH:25]=[C:26]([CH:29]=[CH:30][C:31]=1[O:32][CH3:33])[CH2:27][Cl:28].[ClH:34]>C(C(C)=O)C>[ClH:28].[ClH:34].[C:16]1([CH:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[CH2:8][CH2:9][N:10]2[CH2:11][CH2:12][N:13]([CH2:27][C:26]3[CH:29]=[CH:30][C:31]([O:32][CH3:33])=[C:24]([O:23][CH3:22])[CH:25]=3)[CH2:14][CH2:15]2)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 81740Veratryl chlorideHCID 10356330N-3,3-Diphenylpropylpiperazine

생성물 1

HCID 215378181-(3,3-Diphenylpropyl)-4(3,4-dimethoxybenzyl)piperazine dihydrochloride수율 87.4%

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

N-3,3-Diphenylpropylpiperazine in the amount of 2.8 g (0.01 mole) and 1.87 g (0.01 mole) of 3,4-dimethoxybenzyl chloride were dissolved in 20 ml of methyl ethyl ketone, and the resulting solution was heated at the refluxing temperature for 7.5 hours. After the reaction liquid was left to cool, dry hydrogen chloride gas was passed through the liquid while cooling the liquid to precipitate 1-(3,3-diphenylpropyl)-4-(3,4-dimethoxybenzyl)piperazine dihydrochloride. The crystals of this salt were recrystallized from an ethanol and ether mixed solvent to obtain 4.4 g (87.4% yield) of pure crystals with a melting point of 184°C.

후처리

  1. temperaturethe resulting solution was heated at the refluxing temperature for 7.5 hours
  2. customAfter the reaction liquid
  3. waitwas left
  4. temperatureto cool
  5. temperaturewhile cooling the liquid
  6. customto precipitate 1-(3,3-diphenylpropyl)-4-(3,4-dimethoxybenzyl)piperazine dihydrochloride
  7. customThe crystals of this salt were recrystallized from an ethanol and ether mixed solvent

출처 및 근거

ORD 기록
ord-4c441f7d0045495d8deef7053b50f7a1
출처 데이터셋
uspto-grants-1976_05
특허 번호
US03957790

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