1-(4-Aminobenzoyl)-4-[2-(4-chlorophenyl)ethyl]piperazine → 1-{4-[N-(2-isopropyloxyethyl)amino]benzoyl}-4-[2-(4-chlorophenyl)ethyl]piperazine hydrochloride

HRID 1975342노트

반응식

HRID 1975342 반응식
[NH2:1][C:2]1[CH:24]=[CH:23][C:5]([C:6]([N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][C:16]3[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=3)[CH2:10][CH2:9]2)=[O:7])=[CH:4][CH:3]=1.C1(C)C=CC(S(O[CH2:35][CH2:36][O:37][CH:38]([CH3:40])[CH3:39])(=O)=O)=CC=1>C1(C)C=CC=CC=1>[ClH:22].[CH:38]([O:37][CH2:36][CH2:35][NH:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][C:16]3[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=3)[CH2:10][CH2:9]2)=[O:7])=[CH:23][CH:24]=1)([CH3:40])[CH3:39]

참가 물질

4

반응물 2

HCID 189463571-(4-Aminobenzoyl)-4-[2-(4-chlorophenyl)ethyl]piperazineHCID 190994432-Isopropoxyethyl 4-methylbenzenesulfonate

생성물 1

HCID 190995301-{4-[N-(2-isopropyloxyethyl)amino]benzoyl}-4-[2-(4-chlorophenyl)ethyl]piperazine hydrochloride

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

3.4 g of 1-(4-aminobenzoyl)-4-[2-(4-chlorophenyl)ethyl]piperazine and 2.6 g of 2-isopropyloxyethyl p-toluenesulfonate are suspended in 30 ml of toluene and heated to boiling point. The clear solution so obtained is boiled under reflux for 17 hours and then concentrated by evaporation. Water is added to the residue, and the mixture is rendered alkaline with concentrated sodium hydroxide solution and extracted by shaking with methylene chloride. The crude oil is chromatographed over silica gel and crystallised in the form of the hydrochloride from acetone, yielding 1-{4-[N-(2-isopropyloxyethyl)amino]benzoyl}-4-[2-(4-chlorophenyl)ethyl]piperazine hydrochloride having a melting point of 184°-185°.

후처리

  1. temperatureheated
  2. customThe clear solution so obtained
  3. temperatureunder reflux for 17 hours
  4. concentrationconcentrated by evaporation
  5. additionWater is added to the residue
  6. extractionextracted
  7. customThe crude oil is chromatographed over silica gel
  8. customcrystallised in the form of the hydrochloride from acetone

출처 및 근거

ORD 기록
ord-d5d35f7b41594beca281063b6229749f
출처 데이터셋
uspto-grants-1994_02
특허 번호
US05286728

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