1-Bromo-2-Chloroethane → 1-(4-Chlorobenzyl)-4-(2-chloroethyl)piperazine dihydrochloride

HRID 3832

反応式

HRID 3832 の反応式
[Cl: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.Br[CH2:16][CH2:17][Cl:18]>O1CCCC1>[ClH:1].[ClH:18].[Cl:1][C:2]1[CH:14]=[CH:13][C:5]([CH2:6][N:7]2[CH2:12][CH2:11][N:10]([CH2:16][CH2:17][Cl:18])[CH2:9][CH2:8]2)=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 78491-Bromo-2-ChloroethaneHCID 1348264-Chlorobenzylpiperazine

生成物 1

HCID 123621271-(4-Chlorobenzyl)-4-(2-chloroethyl)piperazine dihydrochloride収率 112%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 15.0 g of 1-(4-chlorobenzyl)piperazine, 14.4 g of 1-bromo-2-chloroethane and 150 ml of tetrahydrofuran was refluxed for 8 hours. The solvent was removed in vacuo, and 2N sodium hydroxide was added to the residue. The product was extracted with methylene chloride, and the extract was dried (sodium sulfate) and concentrated. The salt was precipitated with ethereal hydrochloric acid to give 13.8 g (56% of theory) of 1-(4-chlorobenzyl)-4-(2-chloroethyl)piperazine dihydrochloride as a white crystalline solid.

後処理

  1. temperaturewas refluxed for 8 hours
  2. customThe solvent was removed in vacuo, and 2N sodium hydroxide
  3. additionwas added to the residue
  4. extractionThe product was extracted with methylene chloride
  5. dry with materialthe extract was dried (sodium sulfate)
  6. concentrationconcentrated
  7. customThe salt was precipitated with ethereal hydrochloric acid

出典と根拠

ORDレコード
ord-b5880115943c4665b571bee98c011ee9
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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