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

HRID 1975358
ノート
印刷プレビュー

反応式

HRID 1975358 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 4110039Sodium benzenethiolate2 回HCID 190994641-{4-[N-(2-isopropyloxyethyl)-N-chloroacetylamino]benzoyl}-4-[2-(4-chlorophenyl)ethyl]piperazine fumarate

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-e6dcf6ae5a2e4e4e96b73f56a1d57f61
出典データセット
uspto-grants-1994_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05286728

反応ノート

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