Sodium Carbonate → HCID 20329385, compound

HRID 2057902Notes

Reaction equation

HRID 2057902 reaction equation
Cl[CH:2]([CH3:21])[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:22](=O)([O-])[O-].[Na+].[Na+].[CH3:28][N:29]1[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]1>C(O)C>[CH3:22][N:8]1[C:9](=[O:16])[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[N:5]([C:3](=[O:4])[CH:2]([N:32]2[CH2:33][CH2:34][N:29]([CH3:28])[CH2:30][CH2:31]2)[CH3:21])[C:6]2[N:20]=[CH:19][CH:18]=[CH:17][C:7]1=2

Participants

5

Reactant 3

HCID 10340Sodium CarbonateHCID 531671-MethylpiperazineHCID 20256761HCID 20256761, compound

Product 1

HCID 20329385HCID 20329385, compoundYield 36%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A mixture of 9.5 g of the product of Step A, 3.2 g of sodium carbonate and 4 ml of 1-methyl-piperazine in 120 ml of ethanol was refluxed for 7 hours and the hot solution was then vacuum filtered. The filtrate was evaporated to a volume of about 50 ml and the crystalline precipitate was separated. Then the filtrate was evaporated to dryness in vacuo and the residue was crystallized from isopropanol to obtain a 36% yield of 5,11-dihydro-5-methyl-11-[2-(4-methyl-1-piperazinyl)-propionyl]-6H-pyrido-[2,3-b][1,4]-benzodiazepine-6-one melting at 206°-208° C.

Workup

  1. temperaturewas refluxed for 7 hours
  2. filtrationvacuum filtered
  3. customThe filtrate was evaporated to a volume of about 50 ml
  4. customthe crystalline precipitate was separated
  5. customThen the filtrate was evaporated to dryness in vacuo
  6. customthe residue was crystallized from isopropanol

Sources & evidence

ORD record
ord-97a70a44d0b244b39a25c640ca1b0e3f
Source dataset
uspto-grants-1980_07
Patent number
US04213985

Reaction notes

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