Hydrochloric Acid → 1-(3,3-Diphenylpropyl)-4-(3,4,5-trimethoxybenzyl)piperazine dihydrochloride

HRID 1076784ノート

反応式

HRID 1076784 の反応式
[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]=[C:30]([O:34][CH3:35])[C:31]=1[O:32][CH3:33])[CH2:27][Cl:28].[ClH:36]>C1(C)C=CC=CC=1>[ClH:28].[ClH:36].[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]=[C:30]([O:34][CH3:35])[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

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 774485-(Chloromethyl)-1,2,3-trimethoxybenzeneHCID 10356330N-3,3-Diphenylpropylpiperazine

生成物 1

HCID 215378221-(3,3-Diphenylpropyl)-4-(3,4,5-trimethoxybenzyl)piperazine dihydrochloride収率 80.6%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

N-3,3-Diphenylpropylpiperazine in the amount of 2.8 g (0.01 mole) and 2.2 g (0.01 mole) of 3,4,5-trimethoxybenzyl chloride were dissolved in 20 ml of toluene, and heated at the refluxing temperature for 4.5 hours. After the reaction liquid was left to cool, dry hydrogen chloride gas was passed through the reaction liquid while cooling the liquid to precipitate crystals of 1-(3,3-diphenylpropyl)-4-(3,4,5-trimethoxybenzyl)piperazine dihydrochloride, which were recrystallized from an ethanol and ether mixed solvent to obtain 4.3 g of pure crystals (80.6% yield) with a melting point of 178°C.

後処理

  1. temperatureheated at the refluxing temperature for 4.5 hours
  2. customAfter the reaction liquid
  3. waitwas left
  4. temperatureto cool
  5. temperaturewhile cooling the liquid
  6. customto precipitate crystals of 1-(3,3-diphenylpropyl)-4-(3,4,5-trimethoxybenzyl)piperazine dihydrochloride, which
  7. customwere recrystallized from an ethanol and ether mixed solvent

出典と根拠

ORDレコード
ord-61a6bde97eb94f88a3a73efddef856ca
出典データセット
uspto-grants-1976_05
特許番号
US03957790

反応ノート

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