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

HRID 3841

反応式

HRID 3841 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d30d8a19d77a43a283a0480973ee3168
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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