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Sodium benzenethiolate → 1-[2-(4-Chlorophenyl)ethyl]piperazine

HRID 1975358
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HRID 1975358 반응식
C(O)(=O)/C=C/C(O)=O.C(OCCN(C1C=CC(C([N:26]2[CH2:31][CH2:30][N:29]([CH2:32][CH2:33][C:34]3[CH:39]=[CH:38][C:37]([Cl:40])=[CH:36][CH:35]=3)[CH2:28][CH2:27]2)=O)=CC=1)C(=O)CCl)(C)C.C1([S-])C=CC=CC=1.[Na+]>C(O)C>[Cl:40][C:37]1[CH:38]=[CH:39][C:34]([CH2:33][CH2:32][N:29]2[CH2:28][CH2:27][NH:26][CH2:31][CH2:30]2)=[CH:35][CH:36]=1
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참가 물질

4

반응물 2

HCID 4110039Sodium benzenethiolate2회HCID 190994641-{4-[N-(2-isopropyloxyethyl)-N-chloroacetylamino]benzoyl}-4-[2-(4-chlorophenyl)ethyl]piperazine fumarate

생성물 1

HCID 122357141-[2-(4-Chlorophenyl)ethyl]piperazine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

5 g of 1-{4-[N-(2-isopropyloxyethyl)-N-chloroacetylamino]benzoyl}-4-[2-(4-chlorophenyl)ethyl]piperazine (Example 3) are dissolved in 50 ml of absolute ethanol, and 1.471 g of sodium thiophenolate are added. The mixture is stirred for one hour at room temperature and a further 1 g of sodium thiophenolate is added. The mixture is stirred for a further 3 hours at RT and then the reaction solution is concentrated by evaporation. The oily residue is extracted with ether and the ethereal phases are washed in succession with water, soda solution and water a concentrated by evaporation, and the light-yellow oil is crystallised from ether and hexane, yielding 1-{4-[N-(2-isopropyloxyethyl)-N-phenylmercaptoacetylamino]benzoyl{-4-[2-(4-chlorophenyl)ethyl]piperazine having a melting point of 47°-49°.

후처리

  1. stirringThe mixture is stirred for a further 3 hours at RT
  2. concentrationthe reaction solution is concentrated by evaporation
  3. extractionThe oily residue is extracted with ether
  4. washthe ethereal phases are washed in succession with water, soda solution and water
  5. concentrationa concentrated by evaporation
  6. customthe light-yellow oil is crystallised from ether and hexane

출처 및 근거

ORD 기록
ord-e6dcf6ae5a2e4e4e96b73f56a1d57f61
출처 데이터셋
uspto-grants-1994_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05286728

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