Triethylamine → 3-(4-Benzylpiperazin-1-yl)propanethiol dihydrochloride

HRID 3790

반응식

HRID 3790 반응식
NC(N)=[S:3].[ClH:5].Cl.[CH2:7]([N:14]1[CH2:19][CH2:18][N:17]([CH2:20][CH2:21][CH2:22][Cl:23])[CH2:16][CH2:15]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.C(N(CC)CC)C.[OH-].[Na+]>O.C(O)C>[ClH:23].[ClH:5].[CH2:7]([N:14]1[CH2:19][CH2:18][N:17]([CH2:20][CH2:21][CH2:22][SH:3])[CH2:16][CH2:15]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 2723790ThioureaHCID 13731110Benzyl-4-(3-chloropropyl)piperazine dihydrochloride

생성물 1

HCID 137311143-(4-Benzylpiperazin-1-yl)propanethiol dihydrochloride수율 78%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

15 g of thiourea were added to a solution of 35 g of -benzyl-4-(3-chloropropyl)piperazine dihydrochloride, 20 g of triethylamine and 250 ml of reagent ethanol, and the mixture was refluxed for 8 hours. After the addition of a solution of 10 g of sodium hydroxide in 50 ml of water, the resulting mixture was refluxed for 4 additional hours. The ethanol was removed in vacuo, and water added to the residue which was extracted with methylene chloride, dried (sodium sulfate), and the salt was precipitated with ethereal hydrochloric acid to give 25.1 g (78% of theory) of 3-(4-benzylpiperazin-1-yl)propanethiol dihydrochloride as a white crystalline solid, M.p. 270°-273° C. (dec.).

후처리

  1. temperaturethe mixture was refluxed for 8 hours
  2. temperaturethe resulting mixture was refluxed for 4 additional hours
  3. customThe ethanol was removed in vacuo, and water
  4. additionadded to the residue which
  5. extractionwas extracted with methylene chloride
  6. dry with materialdried (sodium sulfate)
  7. customthe salt was precipitated with ethereal hydrochloric acid

출처 및 근거

ORD 기록
ord-4a99484645cc4c6ca8fde2874eaff9ec
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04722926

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