HCID 12925400, compound → HCID 136302363, compound

HRID 443522Notes

Reaction equation

HRID 443522 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-96834317fd0e4c889c5e5144197807cc
Source dataset
uspto-grants-1981_04
Patent number
US04260758

Reaction notes

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