Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cyclobutylamine | HCID 75645 | — |
| Reactant | HCID 9925711 | HCID 9925711 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 18324820 | HCID 18324820 | 63.5% |
Reaction Steps
A mixture of the hydrobromide salt of Example 12, Step B (6.64 g) and cyclobutylamine (4.15 g) was heated at 90° C. for 1.5 hours. The cooled mixture was diluted with water and extracted with dichloromethane. The extracts were washed with 20% aqueous sodium chloride, dried over anhydrous potassium carbonate and evaporated to a brown oil, which was flash chromatographed on Merck-60 flash silica gel (eluant: hexane-EtOAc 1:1 to remove less polar impurities, followed by dichloromethane-methanol-ammonium hydroxide 95:5:0.1) to provide the title compound (3.08 g, 63.5%), which was used as such in the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06340687B1 |
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| Source dataset | uspto-grants-2002_01 |
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| ORD ID | ord-eb340e370abe401ea6feb69b3c357f2e |
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| Source note | uspto-grants-2002_01 |
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