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 325881ノート

反応式

HRID 325881 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4c57325ab26948bab6d12b87157671a9
出典データセット
uspto-grants-1984_04
特許番号
US04443452

反応ノート

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