Ammonia → HCID 135815261, compound
Reaction equation
[CH3:1][N:2]1[C:10]2[C:9](=[O:11])[NH:8][C:7]([CH2:12][C:13]3[CH:18]=[CH:17][C:16]([NH:19][C:20](=[O:26])/[CH:21]=[CH:22]/OCC)=[CH:15][CH:14]=3)=[N:6][C:5]=2[C:4]([CH2:27][CH2:28][CH3:29])=[N:3]1.N>S(=O)(=O)(O)O>[CH3:1][N:2]1[C:10]2[C:9](=[O:11])[NH:8][C:7]([CH2:12][C:13]3[CH:18]=[C:17]4[C:16](=[CH:15][CH:14]=3)[NH:19][C:20](=[O:26])[CH:21]=[CH:22]4)=[N:6][C:5]=2[C:4]([CH2:27][CH2:28][CH3:29])=[N:3]1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
Concentrated sulphuric acid (10 ml) was added to N-{4-[(1-methyl-7-oxo-3-propyl-6,7-dihydro-1H-pyrazolo[4,3-d]pyrimidin-5-yl)methyl]phenyl}-(E)-3-ethoxy-2-propenamide (980 mg, 0.00248 mol) and the reaction stirred at room temperature for 4 hours. The mixture was then poured carefully onto ice and basified with 0.880 aqueous ammonia solution. The resulting precipitate was filtered and then triturated with boiling acetic acid/water to give the title compound (460 mg), m.p.>300° C.
Workup
- filtrationThe resulting precipitate was filtered
- customtriturated with boiling acetic acid/water
Sources & evidence
- ORD record
- ord-94162da10dcd44dd8977579ad4002016
- Source dataset
- uspto-grants-2001_05
- Patent number
- US06235742B1
Reaction notes
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