Ethanol → 3-[4-(4-Chlorobenzyl)homopiperazin-1-yl]-propanethiol

HRID 3845

반응식

HRID 3845 반응식
NC(N)=[S:3].[Cl:5][C:6]1[CH:23]=[CH:22][C:9]([CH2:10][N:11]2[CH2:17][CH2:16][CH2:15][N:14]([CH2:18][CH2:19][CH2:20]Cl)[CH2:13][CH2:12]2)=[CH:8][CH:7]=1.C(O)C.[OH-].[Na+]>O>[Cl:5][C:6]1[CH:23]=[CH:22][C:9]([CH2:10][N:11]2[CH2:17][CH2:16][CH2:15][N:14]([CH2:18][CH2:19][CH2:20][SH:3])[CH2:13][CH2:12]2)=[CH:8][CH:7]=1

참가 물질

6

반응물 4

HCID 702EthanolHCID 14798Sodium HydroxideHCID 2723790ThioureaHCID 201531881-(4-Chlorobenzyl)-4-(3-chloropropyl)homopiperazine

생성물 1

HCID 201531743-[4-(4-Chlorobenzyl)homopiperazin-1-yl]-propanethiol수율 39.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

4.1 g of thiourea were added to a mixture of 8.0 g of 1-(4-chlorobenzyl)-4-(3-chloropropyl)homopiperazine and 100 ml of reagent ethanol. The mixture was refluxed for 6 hours and then stirred overnight at room temperature. A solution of 5.0 g of sodium hydroxide in 30 ml of water was added, and the resulting solution was refluxed for 4 hours. The ethanol was removed in vacuo, and water was added to the residue. The product was extracted with methylene chloride, and the extract was dried (sodium sulfate) and concentrated to give 3.1 g (39% of theory) of 3-[4-(4-chlorobenzyl)homopiperazin-1-yl]propanethiol as a yellow oil.

후처리

  1. temperatureThe mixture was refluxed for 6 hours
  2. temperaturethe resulting solution was refluxed for 4 hours
  3. customThe ethanol was removed in vacuo, and water
  4. additionwas added to the residue
  5. extractionThe product was extracted with methylene chloride
  6. dry with materialthe extract was dried (sodium sulfate)
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-73e545c91cc447a8af0c692a3811aa45
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04722926

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