Trifluoroacetic acid → HCID 12774391, compound
Reaction equation
S(O)(O)(=O)=O.[NH2:6][N:7]([CH3:11])[C:8]([NH2:10])=[NH:9].[F:12][C:13]([F:18])([F:17])[C:14](O)=O>>[CH3:11][N:7]1[C:8]([NH2:10])=[N:9][C:14]([C:13]([F:18])([F:17])[F:12])=[N:6]1Participants
3
Procedure
1-Amino-1-methyl guanidine sulphate (12.3 g) and trifluoroacetic acid (16 ml) were heated at reflux for 96 h. Excess trifluoroacetic acid was removed by distillation and the residue was basified with sodium bicarbonate and extracted with ethyl acetate. The extract was dried and evaporated to give a white solid (7.2 g) which was recrystallised from a mixture of methyl acetate (8 ml) and petroleum ether (b.p. 60°-80°) (20 ml) to give the title compound as a white powder (5.1 g) m.p. 165°-166°.
Workup
- temperatureat reflux for 96 h
- customExcess trifluoroacetic acid was removed by distillation
- extractionextracted with ethyl acetate
- customThe extract was dried
- customevaporated
Sources & evidence
- ORD record
- ord-0e775d210eed495a89baa205f5aebe85
- Source dataset
- uspto-grants-1987_06
- Patent number
- US04670448
Reaction notes
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