HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → HCID 86710340, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | HCID 86695909 | HCID 86695909 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 86710340 | HCID 86710340 | 84.7% |
Reaction Steps
To a stirred solution of tert-butyl (4-(4-chloro-2-fluorophenyl)-3-formylpyridin-2-yl)carbamate (700 mg, 1.996 mmol) in ethanol (10 mL) at 0° C. was added methylamine (8M in EtOH) (620 mg, 2.49 mL, 19.96 mmol) and the reaction was stirred at rt for 5 h. After the consumption of starting material, solvent was removed under reduced pressure. The residue was washed with hexane (50 mL) and the solid so obtained was dried under vacuum to yield the fluoride salt of 4-((tert-butoxycarbonyl)amino)-8-chloro-6-methylbenzo[c][2,7]naphthyridin-6-ium fluoride (900 mg, 1.69 mmol, 84% yield) as a yellow solid. LC/MS (ESI) m/e 344.2 [(M)+, calcd for C18H19ClN3O2 344.1]; LC/MS retention time (method C): tR=1.90 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08901305B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-88d94bfdfca043b6bad12d0dcf49bb17 |
| Source note | uspto-grants-2014_12 |