N-(4-(4-(Phenylmethyl)-1-piperazinyl)phenyl)acetamide → N-[4-(1-Piperazinyl)phenyl]acetamide

HRID 1087815

反応式

HRID 1087815 の反応式
C1(C[N:8]2[CH2:13][CH2:12][N:11]([C:14]3[CH:19]=[CH:18][C:17]([NH:20][C:21](=[O:23])[CH3:22])=[CH:16][CH:15]=3)[CH2:10][CH2:9]2)C=CC=CC=1>CO.[Pd]>[N:11]1([C:14]2[CH:15]=[CH:16][C:17]([NH:20][C:21](=[O:23])[CH3:22])=[CH:18][CH:19]=2)[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]1

参加物

4

反応物 1

HCID 960610N-(4-(4-(Phenylmethyl)-1-piperazinyl)phenyl)acetamide

生成物 1

HCID 15631761N-[4-(1-Piperazinyl)phenyl]acetamide収率 56%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

This compound was prepared by the hydrogenation of 7.7 (0.025 mole) of N-[4-[4-(phenylmethyl)-1-piperazinyl]phenyl]acetamide in 100 ml of methanol using palladium on carbon as the catalyst. The solution was filtered and the filtrate concentrated under reduced pressure to give an oil which crystallized. The solid was dissolved in a minimum amount of a methylene chloride/10% methanol solution and passed through a 100 g Florisil® column. The desired fractions were concentrated to an oil under reduced pressure which crystallized to give 3.1 g (56%) crude product. A 0.5 g portion was recrystallized from methanol/petroleum ether to give cream colored solid, m.p. 191°-193° C.

後処理

  1. filtrationThe solution was filtered
  2. concentrationthe filtrate concentrated under reduced pressure
  3. customto give an oil which
  4. customcrystallized
  5. dissolutionThe solid was dissolved in a minimum amount of a methylene chloride/10% methanol solution
  6. concentrationThe desired fractions were concentrated to an oil under reduced pressure which
  7. customcrystallized

出典と根拠

ORDレコード
ord-fea3129dcd2645d18642fb590b795be2
出典データセット
uspto-grants-1990_10
特許番号
US04960776

関連ノート

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