HCID 12925400, compound → HCID 136302363, compound

HRID 1577480Notes

Reaction equation

HRID 1577480 reaction equation
[CH2:1]([C:5]1[C:10](=[O:11])[NH:9][N:8]([CH3:12])[C:7]2=[N:13][C:14]([NH2:18])=[N:15][C:16](=[O:17])[C:6]=12)C(C)=O>COCCO>[NH2:18][C:14]1[NH:15][C:16](=[O:17])[C:6]2[CH:5]([CH3:1])[C:10](=[O:11])[NH:9][N:8]([CH3:12])[C:7]=2[N:13]=1

Participants

3

Reactant 1

HCID 12925400HCID 12925400, compound

Product 1

HCID 136302363HCID 136302363, compoundYield 39.7%

Reagents, catalysts & solvents 1

HCID 80192-MethoxyethanolSolvent

Procedure

4-Acetonyl-7-amino-1-methylpyrimido{4,5-c}-pyridazine-3,5-(1H, 2H)-dione (0.054 g) was dissolved in boiling methyl cellosolve (1 l), and the solution was concentrated to 40 ml when precipitated solid was noticed to be present. The mixture was allowed to cool to room temperature and stand overnight. Yellowish-green solid was collected, washed with methyl cellosolve (10 ml) methanol (2 ml), and dried under vacuum at 75° C. to yield 0.018 g (35%) of product: nmr (CF3COOH) δ 3.03(s, 3H), 4.26(s, 3H), 6.83(br s, 2H).

Workup

  1. concentrationthe solution was concentrated to 40 ml when
  2. customprecipitated solid
  3. customYellowish-green solid was collected
  4. washwashed with methyl cellosolve (10 ml) methanol (2 ml)
  5. customdried under vacuum at 75° C.

Sources & evidence

ORD record
ord-8be2a238fdeb4e0ba520c4111da342a1
Source dataset
uspto-grants-1981_09
Patent number
US04288365

Reaction notes

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