HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfoxide → HCID 58977996, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfoxide | HCID 679 | — |
| Reactant | 2-Cyano-3-fluoropyridine | HCID 7060408 | — |
| Reactant | benzyl 2-(methylamino)ethylcarbamate | HCID 10822258 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 58977996 | HCID 58977996 | — |
Reaction Steps
A solution of benzyl 2-(methylamino)ethylcarbamate (prepared as described in example 7, 14 g, 72.1 mmol) in DMSO (20 mL) was reacted with 3-fluoro-2-cyanopyridine (see example 2, 8 g, 65.5 mmol) in a pressure vessel at 85° C. overnight. The resulting mixture was diluted with CHCl3 (100 mL) and added to the top of a silica gel column (150 mm by 7 inches) packed with 20% EtOAc/Hexanes. The column was eluted with a gradient of 20% EtOAc/Hexanes to 100% EtOAc and the clean fractions combined and evaporated to give the product as a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07279487B2 |
| Source dataset | uspto-grants-2007_10 |
| ORD ID | ord-723611520f784b8091e041e461d40331 |
| Source note | uspto-grants-2007_10 |