HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Phosphate, Tribasic → HCID 64387590, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Phosphate, Tribasic | HCID 62657 | — |
| Reactant | 4-Fluorobenzylamine | HCID 67326 | — |
| Reactant | Pyruvic aldehyde dimethyl acetal | HCID 80650 | — |
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 64387590 | HCID 64387590 | 98.1% |
Reaction Steps
4-Fluorobenzylamine (3.00 mL, 26.2 mmol), pyruvic aldehyde dimethyl acetal (3.11 mL, 26.2 mmol), DCE (87 mL), and sodium triacetoxyborohydride (7.79 g, 36.7 mmol) were stirred at ambient temperature. After 14 hours, the reaction was complete as indicated by LCMS. To the reaction mixture was added 30% aqueous K3PO4 (pH=14; 60 mL). The layers were partitioned and the aqueous layer was, extracted with EtOAc (2×50 mL), and washed with brine (60 mL). The organic portion was dried (Na2SO4), filtered, and concentrated to give the title compound (5.83 g, 25.7 mmol, 98% yield). MS (DCI/NH3) m/z 228 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08604053B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-4f1fd2e571d7441a95e01fb136e1b74b |
| Source note | uspto-grants-2013_12 |