Potassium Carbonate → HCID 9798400, compound

HRID 2393738Notes

Reaction equation

HRID 2393738 reaction equation
C(=O)([O-])[O-].[K+].[K+].Br.[NH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]1[CH:18]=[CH:17][C:16]([C:19]2[CH:20]=[CH:21][C:22](=[O:25])[NH:23][N:24]=2)=[CH:15][CH:14]=1.Cl.[C:27](Cl)(=[O:34])[C:28]1[CH:33]=[CH:32][CH:31]=[N:30][CH:29]=1>C(OCC)(=O)C.O1CCCC1>[N:30]1[CH:31]=[CH:32][CH:33]=[C:28]([C:27]([NH:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]2[CH:14]=[CH:15][C:16]([C:19]3[CH:20]=[CH:21][C:22](=[O:25])[NH:23][N:24]=3)=[CH:17][CH:18]=2)=[O:34])[CH:29]=1

Participants

6

Reactant 3

HCID 11430Potassium CarbonateHCID 884383-Pyridinecarbonyl chloride, hydrochloride (1:1)HCID 18977180HCID 18977180, compound

Product 1

HCID 9798400HCID 9798400, compoundYield 60.2%

Reagents, catalysts & solvents 2

HCID 8028TetrahydrofuranSolventHCID 8857Ethyl AcetateSolvent

Procedure

An aqueous solution (25 ml) containing 4.30 g of anhydrous potassium carbonate was added to a suspension in which 2.01 g of 6-[4-(4-aminobutyl)phenyl]pyridazin-3(2H)-one hydrobromide was suspended in ethyl acetate (40 ml) and tetrahydrofuran (10 ml). Under ice cooling, 2.23 g of nicotinic acid chloride hydrochloride was added thereto, and the mixture was stirred for 3 hours. Precipitated crystal was collected by filtration, washed with water, dried and then recrystallized from methanol to obtain 1.30 g of 6-[4-(4-(pyridin-3-ylcarbonylamino)butyl)phenyl]pyridazin-3(2H)-one.

Workup

  1. customPrecipitated crystal
  2. filtrationwas collected by filtration
  3. washwashed with water
  4. customdried
  5. customrecrystallized from methanol

Sources & evidence

ORD record
ord-b36922c81396486eb1a47163529172d9
Source dataset
uspto-grants-1998_09
Patent number
US05808065

Reaction notes

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