Ethyl Acetate → 1-(2-Amino-1-oxo-3-phenylpropyl)-4-(4-fluorophenyl)piperazine hydrochloride

HRID 1106404

反応式

HRID 1106404 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][N:11]([C:14](=[O:31])[CH:15]([NH:23]C(=O)OC(C)(C)C)[CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1.C(OCC)(=O)C.[ClH:38].C(OCC)(=O)C>>[ClH:38].[NH2:23][CH:15]([CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[C:14]([N:11]1[CH2:10][CH2:9][N:8]([C:5]2[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=2)[CH2:13][CH2:12]1)=[O:31]

参加物

4

反応物 3

HCID 8857Ethyl AcetateHCID 21866389Hydrogen chloride-ethyl acetateHCID 538047351,1-Dimethylethyl 2-(4-(4-fluorophenyl)-1-piperazinyl)-2-oxo-1-(phenylmethyl)ethylcarbamate

生成物 1

HCID 185450101-(2-Amino-1-oxo-3-phenylpropyl)-4-(4-fluorophenyl)piperazine hydrochloride収率 96.1%

実験手順

To a solution of 1,1-dimethylethyl 2-(4-(4-fluorophenyl)-1-piperazinyl)-2-oxo-1-(phenylmethyl)ethylcarbamate (2.7 g, 6.3 mmol) in ethyl acetate (20 mmol) under ice-cooling was dropwise added 4N HCl/ethyl acetate (20 ml), and the mixture was stirred at room temperature overnight. The resulting crystals were recovered by filtration and recrystallized from ethanol-diethyl ether to give 1-(2-amino-1-oxo-3-phenylpropyl)-4-(4-fluorophenyl)piperazine hydrochloride (2.2 g, 96.1%) as pale-yellow crystals.

後処理

  1. filtrationThe resulting crystals were recovered by filtration
  2. customrecrystallized from ethanol-diethyl ether

出典と根拠

ORDレコード
ord-4ed625e9de4341d092adb9d460a29452
出典データセット
uspto-grants-2000_05
特許番号
US06057290

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