Hydrochloric Acid → HCID 13853899, compound

HRID 2372349Notes

Reaction equation

HRID 2372349 reaction equation
[CH3:1][O:2][C:3]1[CH:10]=[CH:9][C:6]([CH2:7][NH2:8])=[CH:5][CH:4]=1.[CH3:11][C:12]1[C:13](=[O:22])[N:14]([CH:19]([CH3:21])[CH3:20])[N:15]=[CH:16][C:17]=1Cl.C(=O)([O-])O.[Na+].C(=O)([O-])[O-].[K+].[K+].C(N(CCC)CCC)CC.Cl>>[CH3:11][C:12]1[C:13](=[O:22])[N:14]([CH:19]([CH3:20])[CH3:21])[N:15]=[CH:16][C:17]=1[NH:8][CH2:7][C:6]1[CH:9]=[CH:10][C:3]([O:2][CH3:1])=[CH:4][CH:5]=1

Participants

7

Reactant 6

HCID 313Hydrochloric AcidHCID 7616TripropylamineHCID 11430Potassium CarbonateHCID 754524-MethoxybenzylamineHCID 516892Sodium BicarbonateHCID 13853845HCID 13853845, compound

Product 1

HCID 13853899HCID 13853899, compound

Conditions

Temperature
150 °C

Procedure

A mixture comprising 2.2 g of 4-methoxybenzylamine, 0.30 g of 4-methyl-5-chloro-2-i-propyl-3(2H)pyridazinone, 1.34 g of sodium hydrogencarbonate, 0.23 g of potassium carbonate and 5 ml of tri-n-propylamine, was heated at 150° C. for 18 hours. The reaction mixture was acidified with a 10% hydrochloric acid aqueous solution, and extracted with 60 ml of benzene. The benzene layer was washed with water, and dried over anhydrous sodium sulfate, and then the solvent was distilled off to obtain an oily substance. This substance was crystallized from 5 ml of ethyl ether to obtain 40 mg of the above identified compound.

Workup

  1. extractionextracted with 60 ml of benzene
  2. washThe benzene layer was washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationthe solvent was distilled off
  5. customto obtain an oily substance
  6. customThis substance was crystallized from 5 ml of ethyl ether
  7. customto obtain 40 mg of the

Sources & evidence

ORD record
ord-99f1c15da5034abab4866b56829a1836
Source dataset
uspto-grants-1992_03
Patent number
US05098900

Reaction notes

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