Potassium Carbonate → 1-[4-(3-Ethoxypropylamino)benzoyl]-4-[2-(4-chlorophenyl)ethyl]piperazine

HRID 1975346노트

반응식

HRID 1975346 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.[CH2:25]([O:27][CH2:28][CH2:29][CH2:30]Br)[CH3:26].C([O-])([O-])=O.[K+].[K+]>C(O)(C)C>[CH2:25]([O:27][CH2:28][CH2:29][CH2:30][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)[CH3:26]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 2604931-bromo-3-ethoxypropaneHCID 189463571-(4-Aminobenzoyl)-4-[2-(4-chlorophenyl)ethyl]piperazine

생성물 1

HCID 190994271-[4-(3-Ethoxypropylamino)benzoyl]-4-[2-(4-chlorophenyl)ethyl]piperazine

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

11 g of 1-(4-aminobenzoyl)-4-[2-(4-chlorophenyl)ethyl]piperazine and 5.7 g of 3-ethoxypropyl bromide are suspended in 150 ml of isopropanol and dissolved at 100°. 9.4 g of potash are added thereto, and the mixture is boiled under reflux for 20 hours. Concentration by evaporation and chromatography over silica gel yield an oil, which is crystallised from methylene chloride and petroleum ether, yielding 1-[4-(3-ethoxypropylamino)benzoyl]-4-[2-(4-chlorophenyl)ethyl]piperazine having a melting point of 87°-89°.

후처리

  1. dissolutiondissolved at 100°
  2. temperatureunder reflux for 20 hours
  3. concentrationConcentration
  4. customby evaporation and chromatography over silica gel
  5. customyield an oil, which
  6. customis crystallised from methylene chloride and petroleum ether

출처 및 근거

ORD 기록
ord-8e0152fa8b7a4eda9ce8432ef410d20a
출처 데이터셋
uspto-grants-1994_02
특허 번호
US05286728

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