HuagongsheHuagongshe Chemistry Print Report · For research reference only
Boron trifluoride → HCID 11211410, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Boron trifluoride | HCID 6356 | — |
| Reactant | Benzyl 7-(diethoxyphosphoryl)-3,7-diazabicyclo[4.1.0]heptane-3-carboxylate | HCID 59455678 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 11211410 | HCID 11211410 | 17% |
Reaction Steps
BF3 etherate (3.10 mL, 24.4 mmol) was added to a solution of benzyl 7-(diethoxyphosphoryl)-3,7-diazabicyclo[4.1.0]heptane-3-carboxylate (3.00 g, 8.14 mmol; Example H, step D) in DCM (10 mL) at 0° C. The resulting solution was warmed to room temperature and stirred at room temperature for 3 days. The solvent was removed in vacuo, ethyl acetate (30 mL) and saturated sodium bicarbonate (20 mL) were added. The organic layer was separated, dried (sodium sulfate) and concentrated in vacuo. The residue obtained was purified by flash chromatography on silica gel (ethyl acetate) to give trans-benzyl 3-(diethoxyphosphorylamino)-4-fluoropiperidine-1-carboxylate (0.53 g, 17%) as oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08981085B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-2ed4f62a95114004af737f9dea010594 |
| Source note | uspto-grants-2015_03 |