Triethylamine → 1-Cinnamyl-4-(3-chloropropyl)piperazine dihydrochloride

HRID 3841

반응식

HRID 3841 반응식
[CH2:1](Br)[CH:2]=[CH:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.O.Cl.Cl.[Cl:14][CH2:15][CH2:16][CH2:17][N:18]1[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1.[Cl:24]CCCN1CCNCC1.Cl.Cl.C(N(CC)CC)C>C(O)C>[ClH:14].[ClH:24].[CH2:1]([N:21]1[CH2:22][CH2:23][N:18]([CH2:17][CH2:16][CH2:15][Cl:14])[CH2:19][CH2:20]1)[CH:2]=[CH:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 98116BromomethylstyreneHCID 131714940Bis(1-(3-chloropropyl)piperazine);hydrate;tetrahydrochloride

생성물 1

HCID 704154971-Cinnamyl-4-(3-chloropropyl)piperazine dihydrochloride수율 278.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

6.0 g of cinnamyl bromide were added to a mixture of 7.4 g of 1-(3-chloropropyl)piperazine dihydrochloride hemihydrate, 6.1 g of triethylamine and 100 ml of reagent ethanol. The mixture was refluxed for 4 hours and then stirred overnight. After removal of the solvent in vacuo, water was added to the residue. The product was then extracted with ether and the extract was dried (magnesium sulfate) and concentrated. The resulting oil was chromatographed on silica gel (methylene chloride/methanol: 9/1) and precipitated with ethereal hydrochloric acid to give 7.4 g (70% of theory) of 1-cinnamyl-4-(3-chloropropyl)piperazine dihydrochloride.

후처리

  1. temperatureThe mixture was refluxed for 4 hours
  2. customAfter removal of the solvent in vacuo, water
  3. additionwas added to the residue
  4. extractionThe product was then extracted with ether
  5. dry with materialthe extract was dried (magnesium sulfate)
  6. concentrationconcentrated
  7. customThe resulting oil was chromatographed on silica gel (methylene chloride/methanol: 9/1)
  8. customprecipitated with ethereal hydrochloric acid

출처 및 근거

ORD 기록
ord-d30d8a19d77a43a283a0480973ee3168
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04722926

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