HCID 12925400, compound → HCID 136302363, compound
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]=1Participants
3
Reactant 1
Product 1
Reagents, catalysts & solvents 1
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
- concentrationthe solution was concentrated to 40 ml when
- customprecipitated solid
- customYellowish-green solid was collected
- washwashed with methyl cellosolve (10 ml) methanol (2 ml)
- customdried under vacuum at 75° C.
Sources & evidence
- ORD record
- ord-bb0e8a0839e34520852c0176667bf5a5
- Source dataset
- uspto-grants-1980_12
- Patent number
- US04237289
Reaction notes
Loading…