HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 131724510, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 23502528 | HCID 23502528 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 131724510 | HCID 131724510 | 75.8% |
Reaction Steps
4-Chloro-3-[7-fluoro-5-(2-chloropropionylamino)-2H-1,4-benzoxazine-3(4H)-on-6yl]-1-methyl-5-difluoromethoxy-1H-pyrazole (300 mg, 0.66 mmol) was dissolved in anhydrous dimethylformamide (10 ml) and solution stirred under ice-cooling. Sodium hydride (20 mg, 95%, 0.79 mmol) was added slowly in portions and solution stirred at room temperature for 2 hr. Solution was then added to ice-water and product extracted with ethyl acetate. Evaporation of the solvent afforded a residue which was purified by flash chromatography on silica gel in hexane-ethyl acetate (1:1) to furnish the title compound (209.2 mg, 0.50 mmol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06770596B1 |
| Source dataset | uspto-grants-2004_08 |
| ORD ID | ord-4b24f6fc3fb340b48649ef640a0125fa |
| Source note | uspto-grants-2004_08 |