Methane → HCID 70240816, compound
Reaction equation
CS(O)(=O)=O.[CH2:6]([O:9][C:10]1[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=1[C:12]([NH2:14])=[NH:13])[CH2:7][CH3:8].S(O)(O)(=O)=O.N[C:25]1[C:29]([C:30](N)=[O:31])=[CH:28][NH:27][N:26]=1.C([O-])(=O)C.[Na+].C>[OH-].[Na+].C(O)(=O)C>[CH2:6]([O:9][C:10]1[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=1[CH:12]1[N:14]=[C:28]2[N:27]=[N:26][CH:25]=[C:29]2[C:30](=[O:31])[NH:13]1)[CH2:7][CH3:8]Participants
7
Conditions
- Temperature
- 180 °C
Procedure
A stirred mixture of 2-propoxybenzamidine methane-sulphonate (1.0 g), 3-amino-4-pyrazole-carboxamide sulphate (0.5 g) and sodium acetate (0.82 g) was heated in an oil bath (180° C.) for one hour. The reaction mixture was dissolved in hot 2 Normal sodium hydroxide (10 ml) and the solution was treated with charcoal and neutralised with glacial acetic acid. A precipitate was collected, washed with water and eluted from a silica column with chloroform. The combined fractions containing product were evaporated to dryness to afford the title compound, 148 mg, m.p. 182-183.5° C.
Workup
- customA precipitate was collected
- washwashed with water
- washeluted from a silica column with chloroform
- additionThe combined fractions containing product
- customwere evaporated to dryness
Sources & evidence
- ORD record
- ord-5f0fe3630168412db24bc51ce8800b47
- Source dataset
- uspto-grants-2001_03
- Patent number
- US06200980B1
Reaction notes
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