Methylamine → HCID 15079195, compound

HRID 973402Notes

Reaction equation

HRID 973402 reaction equation
CO[C:3]1[C:12]2[C:7](=[CH:8][C:9]([C:13]3[CH:14]([CH3:20])[CH2:15][C:16](=[O:19])[NH:17][N:18]=3)=[CH:10][CH:11]=2)[N:6]=[C:5]([CH3:21])[N:4]=1.[CH3:22][NH2:23]>CO>[CH3:20][CH:14]1[C:13]([C:9]2[CH:8]=[C:7]3[C:12]([C:3]([NH:23][CH3:22])=[N:4][C:5]([CH3:21])=[N:6]3)=[CH:11][CH:10]=2)=[N:18][NH:17][C:16](=[O:19])[CH2:15]1

Participants

4

Reactant 2

HCID 6329MethylamineHCID 15079193HCID 15079193, compound

Product 1

HCID 15079195HCID 15079195, compoundYield 76%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

In 20 ml of 40% methylamine solution in methanol was suspended 0.50 g of Compound 63 obtained in Example 65. The suspension was heated under reflux with stirring for 4 hours and then concentrated. The residue was subjected to partition between water and chloroform, and the organic layer was dried and concentrated. The residue was crystallized from a mixture of dimethylformamide and water to give 0.38 g (76%) of 4,5-dihydro-5-methyl-6-(4-methylamino2-methylquinazolin-7-yl)-3(2H)-pyridazinone (Compound 64).

Workup

  1. temperatureThe suspension was heated
  2. temperatureunder reflux
  3. concentrationconcentrated
  4. customto partition between water and chloroform
  5. customthe organic layer was dried
  6. concentrationconcentrated
  7. customThe residue was crystallized from a mixture of dimethylformamide and water

Sources & evidence

ORD record
ord-8b38afa3b2a94eb684c663dd08ebd557
Source dataset
uspto-grants-1991_11
Patent number
US05063227

Reaction notes

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