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

HRID 1975342ノート

反応式

HRID 1975342 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-d5d35f7b41594beca281063b6229749f
出典データセット
uspto-grants-1994_02
特許番号
US05286728

反応ノート

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