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

HRID 1975346ノート

反応式

HRID 1975346 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.[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-8e0152fa8b7a4eda9ce8432ef410d20a
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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