Toluene → 1-acetyl-3-{3-[4-(diphenylmethyl)-1-piperazinyl]propyl}-1,3-dihydro-2H-benzimidazol-2-one

HRID 354997

반응식

HRID 354997 반응식
C(O[C:5](=[O:7])[CH3:6])(=O)C.[C:8]1([CH:14]([C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)[N:15]2[CH2:20][CH2:19][N:18]([CH2:21][CH2:22][CH2:23][N:24]3[C:28]4[CH:29]=[CH:30][CH:31]=[CH:32][C:27]=4[NH:26][C:25]3=[O:33])[CH2:17][CH2:16]2)[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.CC1C=CC=CC=1>O>[C:5]([N:26]1[C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=2[N:24]([CH2:23][CH2:22][CH2:21][N:18]2[CH2:19][CH2:20][N:15]([CH:14]([C:8]3[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=3)[C:34]3[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=3)[CH2:16][CH2:17]2)[C:25]1=[O:33])(=[O:7])[CH3:6]

참가 물질

5

반응물 3

HCID 1140TolueneHCID 4615OxatomideHCID 7918Acetic Anhydride

생성물 1

HCID 131055881-acetyl-3-{3-[4-(diphenylmethyl)-1-piperazinyl]propyl}-1,3-dihydro-2H-benzimidazol-2-one

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 1.55 parts of acetic acid anhydride, 3 parts of 1-{3-[4-(diphenylmethyl)-1-piperazinyl]propyl}-1,3-dihydro-2H-benzimidazol-2-one and 22.5 parts of methylbenzene is stirred and refluxed overnight. Water is added to the reaction mixture and the layers are separated. The organic phase is dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions are collected and the eluent is evaporated, yielding 1-acetyl-3-{3-[4-(diphenylmethyl)-1-piperazinyl]propyl}-1,3-dihydro-2H-benzimidazol-2-one; mp. 124.4° C.

후처리

  1. temperaturerefluxed overnight
  2. customthe layers are separated
  3. customThe organic phase is dried
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue is purified by column-chromatography over silica gel using
  7. additiona mixture of trichloromethane and methanol (95:5 by volume) as eluent
  8. customThe pure fractions are collected
  9. customthe eluent is evaporated

출처 및 근거

ORD 기록
ord-aad8a92e033a43599bf0eefee954b6b3
출처 데이터셋
uspto-grants-1983_03
특허 번호
US04377578

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