HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Fluorobenzylamine → HCID 10405113, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Fluorobenzylamine | HCID 67326 | — |
| Reactant | Benzyl 4-oxopiperidine-1-carboxylate | HCID 643496 | — |
| Reactant | Sodium cyanoborohydride | HCID 5003444 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 10405113 | HCID 10405113 | 60% |
Reaction Steps
A solution of 4-fluorobenzylamine (5.48 g, 43.8 mmol) in a mixture of methanol and acetic acid (5:1, 60 mL) was added dropwise to a solution of benzyl 4-oxo-1-piperidine carboxylate (10.2 g, 43.8 mmol) in methanol (150 mL) at rt. To this mixture sodium cyanoborohydride (5.50 g, 87.5 mmol) was slowly added. After 20 hours stirring at rt the reaction mixture was neutralized and the solvent was removed by evaporation under reduced pressure. The residue was partitioned between dichloromethane and water. The organic layer was dried over sodium sulphate, filtered and evaporated to dryness. Purification of the residue by silica gel column chromatography, eluting with 7% methanol in dichloromethane, afforded the desired compound (9.0 g, 60%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07253186B2 |
| Source dataset | uspto-grants-2007_08 |
| ORD ID | ord-34f4a452843842368d0693f8b0c2a480 |
| Source note | uspto-grants-2007_08 |