Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | O-Methylhydroxylamine hydrochloride | HCID 521874 | — |
| Reactant | HCID 18770570 | HCID 18770570 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178502904 | HCID 178502904 | 0.7% |
Reaction Steps
169.2 mg (20 mMol) O-methylhydroxylamine hydrochloride and 2.0 g (8.3 mMol) S-methyl-N-cyano-N′-(6-chloropyrid-3-yl)isothiourea are added to 50 ml ethanol and treated with 1.27 ml (9.1 mMol) triethylamine and 50.0 ml water. The reaction mixture is then stirred for ca. 18 hours at 60° C. under a protective gas (argon). At the end of the reaction the ethanol is distilled off under reduced pressure and the aqueous residue is extracted three times with chloroform. After drying the organic phase is evaporated to dryness under reduced pressure and the residue is purified by preparative HPLC. 13.5 mg (0.7%) N-methoxyamino-N′-(6-chloropyrid-3-yl)cyanoguanidine are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07763640B2 |
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| Source dataset | uspto-grants-2010_07 |
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| ORD ID | ord-78bec9b78c7f481cb3da3131299dcf2d |
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| Source note | uspto-grants-2010_07 |
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