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

HRID 1087815

반응식

HRID 1087815 반응식
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

참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fea3129dcd2645d18642fb590b795be2
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04960776

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