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

HRID 3832

반응식

HRID 3832 반응식
[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

참가 물질

4

반응물 2

HCID 78491-Bromo-2-ChloroethaneHCID 1348264-Chlorobenzylpiperazine

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b5880115943c4665b571bee98c011ee9
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04722926

연결된 노트

불러오는 중…