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Potassium Carbonate → 6H-Pyrido(2,3-b)(1,4)benzodiazepin-6-one, 5,11-dihydro-11-((4-(2,2-dimethylpropyl)-1-piperazinyl)acetyl)-

HRID 2057980
Notes
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Reaction equation

HRID 2057980 reaction equation
Cl[CH2:2][C:3]([N:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[C:9](=[O:16])[NH:8][C:7]2[CH:17]=[CH:18][CH:19]=[N:20][C:6]1=2)=[O:4].C(=O)([O-])[O-].[K+].[K+].[CH3:27][C:28]([CH3:37])([CH3:36])[CH2:29][N:30]1[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]1>C(O)C>[CH3:27][C:28]([CH3:37])([CH3:36])[CH2:29][N:30]1[CH2:35][CH2:34][N:33]([CH2:2][C:3]([N:5]2[C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=3[C:9](=[O:16])[NH:8][C:7]3[CH:17]=[CH:18][CH:19]=[N:20][C:6]2=3)=[O:4])[CH2:32][CH2:31]1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 12005311-(Chloroacetyl)-5,11-dihydro-6H-pyrido(2,3-b)(1,4)benzodiazepin-6-oneHCID 167489111-(2,2-Dimethylpropyl)piperazine

Product 1

HCID 30532156H-Pyrido(2,3-b)(1,4)benzodiazepin-6-one, 5,11-dihydro-11-((4-(2,2-dimethylpropyl)-1-piperazinyl)acetyl)-

Reagents, catalysts & solvents 1

HCID 702
Ethanol
Solvent

Procedure

7.15 gm of 11-chloroacetyl-5,11-dihydro-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one, 2.9 gm of potassium carbonate and 4.5 gm of 1-(2,2-dimethyl-propyl)-piperazine were refluxed for 5 hours in 100 ml of absolute ethanol. Then, the hot reaction mixture was suction filtered. The crystals which precipitated out of the filtrate were then recrystallized from isopropanol in the presence of activated charcoal.

Workup

  1. filtrationfiltered
  2. customThe crystals which precipitated out of the filtrate
  3. customwere then recrystallized from isopropanol in the presence of activated charcoal

Sources & evidence

ORD record
ord-16f3293d61954c109dad5a2dab1aefe1
Source dataset
uspto-grants-1980_07
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US04213984

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes