Sodium Carbonate → 5,10-Dihydro-5-{[N-methyl-N-(1-methyl-4-piperidinyl)amino]carbonyl}-11H-dibenzo[b,e][1,4]diazepin-11-one

HRID 325881노트

반응식

HRID 325881 반응식
Cl[C:2]([N:4]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[C:8](=[O:15])[NH:7][C:6]2[CH:16]=[CH:17][CH:18]=[CH:19][C:5]1=2)=[O:3].C(=O)([O-])[O-].[Na+].[Na+].[CH3:26][N:27]1[CH2:32][CH2:31][CH:30]([NH:33][CH3:34])[CH2:29][CH2:28]1>C(#N)C>[CH3:34][N:33]([C:2]([N:4]1[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=2[C:8](=[O:15])[NH:7][C:6]2[CH:16]=[CH:17][CH:18]=[CH:19][C:5]1=2)=[O:3])[CH:30]1[CH2:31][CH2:32][N:27]([CH3:26])[CH2:28][CH2:29]1

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 5663231-Methyl-4-(methylamino)piperidineHCID 132767455-chlorocarbonyl-5,10-dihydro-11H-dibenzo[b,e][1,4]diazepin-11-one

생성물 1

HCID 132767465,10-Dihydro-5-{[N-methyl-N-(1-methyl-4-piperidinyl)amino]carbonyl}-11H-dibenzo[b,e][1,4]diazepin-11-one

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Nine grams (0.033 mol) of 5-chlorocarbonyl-5,10-dihydro-11H-dibenzo[b,e][1,4]diazepin-11-one, 5.3 gm (0.05 mol) of sodium carbonate, and 5.2 gm (0.036 mol) of 1-methyl-4-methylamino-piperidine were refluxed in 150 ml of acetonitrile for 15 minutes under stirring. The mixture was filtered while hot, and then the filtrate was placed on a silica gel column and eluted first with acetonitrile and then with a methylene chloride/ethyl acetate/cyclohexane/methanol/ammonia (175:75:23:23:3) mixture. The desired fraction was concentrated by evaporation in vacuo, and the residue was recrystallized from acetonitrile.

후처리

  1. filtrationThe mixture was filtered while hot, and then the filtrate
  2. washeluted first with acetonitrile
  3. concentrationThe desired fraction was concentrated by evaporation in vacuo
  4. customthe residue was recrystallized from acetonitrile

출처 및 근거

ORD 기록
ord-4c57325ab26948bab6d12b87157671a9
출처 데이터셋
uspto-grants-1984_04
특허 번호
US04443452

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