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

HRID 3832

Reaktionsgleichung

Reaktionsgleichung von HRID 3832
[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

Komponenten

4

Edukt 2

HCID 78491-Bromo-2-ChloroethaneHCID 1348264-Chlorobenzylpiperazine

Produkt 1

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

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-b5880115943c4665b571bee98c011ee9
Quelldatensatz
uspto-grants-1988_02
Patentnummer
US04722926

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