HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cyanomethylenetributylphosphorane → HCID 118030927, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cyanomethylenetributylphosphorane | HCID 4622928 | — |
| Reactant | HCID 67991756 | HCID 67991756 | — |
| Reactant | HCID 118020513 | HCID 118020513 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 118030927 | HCID 118030927 | — |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
To a solution of [(2S,4S)-2-(hydroxymethyl)-4-methyl-1,3-oxazinan-3-yl][5-methyl-2-(2H-1,2,3-triazol-2-yl)phenyl]methanone obtained in Reference Example 17 (0.070 g, 0.22 mmol) in toluene (1 mL), 5-fluoro-2-(1H-pyrazol-4-yl)pyridine obtained in Reference Example 11 (0.040 g, 0.24 mmol) and cyanomethylene tributylphosphorane (0.087 mL, 0.33 mmol) were added, and the resulting mixture was stirred with heating for 3 hours at 100° C. The solvent was distilled off under reduced pressure, and the obtained residue was purified by column chromatography (KP-NH 12 g, hexane/EtOAc=80/20 to 0/100) (HP-Sil 10 g, hexane/EtOAc=80/20 to 0/100) to obtain the title compound (0.11 g) (colorless oil).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09266870B2 |
| Source dataset | uspto-grants-2016_02 |
| ORD ID | ord-67d52c81ab7a4e5ea6e85ae649707a83 |
| Source note | uspto-grants-2016_02 |