Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cyanogen Bromide | HCID 10476 | — |
| Reactant | HCID 66930092 | HCID 66930092 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 66930368 | HCID 66930368 | — |
Reaction Steps
C-(5,6-Dimethoxypyridazin-3-yl)methylamine trifluoroacetic acid salt (37 mg) was initially charged in a mixture of ethanol and water (3.75/0.75 ml) while stirring at RT. Thereafter, cyanogen bromide solution (0.1 ml; 5M in ACN) was cautiously added dropwise and the mixture was stirred at RT for 3 h. Then further cyanogen bromide solution (0.1 ml) was added and the mixture was left to stand overnight. After again adding cyanogen bromide solution (0.1 ml), the mixture was stirred for 4 h, left to stand over the weekend and then heated to 40° C. for 2 h. Subsequently, the solvent was drawn off and the residue was purified by means of preparative HPLC. The product-containing fractions were combined, freed of the acetonitrile and freeze-dried. 18 mg of the desired compound were obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08598177B2 |
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| Source dataset | uspto-grants-2013_12 |
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| ORD ID | ord-6fbe136973214f619a5c9a6f7adbad99 |
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| Source note | uspto-grants-2013_12 |
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