HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → HCID 86673553, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | HCID 86673554 | HCID 86673554 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 86673553 | HCID 86673553 | 75.9% |
Reaction Steps
In a dry reaction bottle, 16 g (R)-1-[2-formyloxy-5-nitro-6-chloropyridin-4-yl]piperidine-3-carbamic acid tert-butyl ester (40 mmol) was added and dissolved in 50 mL ethanol. 31 g 40% methylamine aqueous solution (400 mmol) was added. The stirring was continued for 2 days at 60° C. The reaction solution was extracted with dichloromethane, dried, and evaporated to dryness to afford a crude product as yellow solid, which was purified through a column chromatography (ethyl acetate:petroleum ether=1:1) to afford 12 g titled product with a yield of 75.9%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08680089B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-7327c7e771ff4f31985e13b196adc988 |
| Source note | uspto-grants-2014_03 |