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

HRID 2057978Notes

Reaction equation

HRID 2057978 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-].[Na+].[Na+].[CH3:27][C:28](=[CH2:36])[CH2:29][N:30]1[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]1>C(O)C>[CH3:36][C:28](=[CH2:27])[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

Participants

5

Procedure

8.62 gm of 11-chloroacetyl-5,11-dihydro-6H-pyrido[2,3-b][1,4]-benzodiazepin-6-one, 3.5 gm of sodium carbonate and 4.6 gm of 1-(2-methyl-allyl)-piperazine were refluxed in 100 ml of absolute ethanol for 2 hours. Then, the reaction mixture was suction-filtered while still hot, and the filtrate was evaporated to a volume of 40 ml and cooled. The precipitated crystals were recrystallized from ethanol in the presence of activated charcoal, yielding 75% of theory of the compound of the formula ##STR9## which had a melting point of 205°-207° C.

Workup

  1. filtrationThen, the reaction mixture was suction-filtered while still hot, and the filtrate
  2. customwas evaporated to a volume of 40 ml
  3. temperaturecooled
  4. customThe precipitated crystals were recrystallized from ethanol in the presence of activated charcoal
  5. customyielding 75% of theory of the compound of the formula ##STR9## which

Sources & evidence

ORD record
ord-1f642717ea274dd491406a70edbbae38
Source dataset
uspto-grants-1980_07
Patent number
US04213984

Reaction notes

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