Sodium Carbonate → HCID 20332025, compound

HRID 2057388Notes

Reaction equation

HRID 2057388 reaction equation
[Cl:1][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][N:28]1[CH2:34][CH2:33][CH2:32][NH:31][CH2:30][CH2:29]1>C(O)C>[ClH:1].[ClH:1].[CH3:27][N:28]1[CH2:34][CH2:33][CH2:32][N:31]([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])[CH2:30][CH2:29]1

Participants

5

Reactant 3

HCID 10340Sodium CarbonateHCID 12005311-(Chloroacetyl)-5,11-dihydro-6H-pyrido(2,3-b)(1,4)benzodiazepin-6-oneHCID 2283491-Methylhomopiperazine

Product 1

HCID 20332025HCID 20332025, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

8.6 gm of 11-chloroacetyl-5,11-dihydro-6H-pyrido[2,3-b][1,4]benzodiazepin-6-one, 3.5 gm of sodium carbonate and 4.5 gm of hexahydro-1-methyl-1H-1, 4-diazepine were refluxed in 100 ml of ethanol for 2.5 hours. Then the hot mixture was suction-filtered, the alcohol was distilled off, and the residue was triturated with dioxane. The precipitated crystals were dissolved in ethanol and converted into the dihydrochloride by addition of concentrated hydrochloric acid. After recrystallization from 94% ethanol:

Workup

  1. filtrationThen the hot mixture was suction-filtered
  2. distillationthe alcohol was distilled off
  3. customthe residue was triturated with dioxane
  4. dissolutionThe precipitated crystals were dissolved in ethanol
  5. additionconverted into the dihydrochloride by addition of concentrated hydrochloric acid
  6. customAfter recrystallization from 94% ethanol

Sources & evidence

ORD record
ord-173ee14f1c824f21a53048b4f5f37ce9
Source dataset
uspto-grants-1980_07
Patent number
US04210648

Reaction notes

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