Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | HCID 68675669 | HCID 68675669 | — |
| Reactant | methyl N-(3,5-diamino-6-chloropyrazine-2-carbonyl)carbamimidothioate;hydroiodide | HCID 140329753 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | Ammonia | HCID 222 | — |
| Product | HCID 178512164 | HCID 178512164 | — |
Reaction Steps
5-[4-(5-Amino-pentyl)-piperazin-1-yl]pentylamine trifluoroacetate (Intermediate P) (172 mg, 0.24 mmol) is added to a stirring solution of 1-(3,5-diamino-6-chloro-pyrazine-2-carbonyl)-2-methyl-isothiourea hydroiodide (93 mg, 0.48 mmol) in DMF (1 mL). The resulting mixture is heated to 50° C. for 8 hours and then allowed to cool to RT. The reaction mixture is quenched with 5% citric acid solution and addition of DCM results in the formation of a gum. The gum is isolated and dissolved in MeOH (2 mL). The solution is passed through a “capture release” SCX-2 cartridge eluting with 1 N ammonia in MeOH followed by 1:1 MeOH:ammonia solution to afford the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07803804B2 |
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| Source dataset | uspto-grants-2010_09 |
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| ORD ID | ord-8bb354001b224cad9e29741dab652d8e |
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| Source note | uspto-grants-2010_09 |
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