HCID 15079120, compound → HCID 178429553, compound

HRID 973404Notes

Reaction equation

HRID 973404 reaction equation
[CH3:1][CH:2]1[C:7]([C:8]2[CH:17]=[C:16]3[C:11]([C:12](SC)=[N:13][CH:14]=[N:15]3)=[CH:10][CH:9]=2)=[N:6][NH:5][C:4](=[O:20])[CH2:3]1>CN(C)C=O.[Ni]>[N:15]1[C:16]2[C:11](=[CH:10][CH:9]=[C:8]([C:7]3[CH:2]([CH3:1])[CH2:3][C:4](=[O:20])[NH:5][N:6]=3)[CH:17]=2)[CH2:12][NH:13][CH:14]=1

Participants

4

Reactant 1

HCID 15079120HCID 15079120, compound

Product 1

HCID 178429553HCID 178429553, compoundYield 26%

Reagents, catalysts & solvents 2

HCID 935NickelCatalystHCID 6228DimethylformamideSolvent

Conditions

Temperature
60 °C

Procedure

In 10 ml of dimethylformamide was dissolved 1.0 g of Compound 57 obtained in Example 19, and 5.0 g of Raney nickel was added to the solution, followed by stirring at 60° C. for 1 hour. The catalyst was filtered off, and the filtrate was concentrated. Water was added to the residue, and the crystals precipitated were collected by filtration and dried to give 0.22 g (26%) of 4,5-dihydro-6-(3,4-dihydroquinazolin-7-yl)-5-methyl-3(2H)-pyridazinone (Compound 71).

Workup

  1. additionwas added to the solution
  2. filtrationThe catalyst was filtered off
  3. concentrationthe filtrate was concentrated
  4. additionWater was added to the residue
  5. customthe crystals precipitated
  6. filtrationwere collected by filtration
  7. customdried

Sources & evidence

ORD record
ord-777971f8dc7449a188b65461eed2f271
Source dataset
uspto-grants-1991_11
Patent number
US05063227

Reaction notes

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