HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 18519629, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Carbonate Ion | HCID 19660 | — |
| Reactant | Ethyl 2-bromopropionate | HCID 79040 | — |
| Reactant | HCID 18519625 | HCID 18519625 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 18519629 | HCID 18519629 | 5.3% |
Reaction Steps
Step 3 A mixture of 4-chloro-3-(2-amino-4-chloro-6-fluoro-3-hydroxyphenyl)-5-difluoromethoxy-1-methyl-1H-pyrazole (0.88 g), ethyl 2-bromopropionate (0.70 g) and potassiun carbonate (0.711 g) in acetonitrile (30 ml) was stirred overnight at ambient temperature. The reaction mixture was poured into water and extracted with ethyl acetate. The organic phase was washed with brine (×3) and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure and the oily product was subjected to silica gel chromatography eluted with ethyl acetate and hexane (1:4) to afford 4-chloro-3-(8-chloro-6-fluoro-2-methyl-2H-1,4-benzoxazine-3-one-5-yl)-5-difluoromethoxy-1-methyl-1H-pyrazole (0.054 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06573218B1 |
| Source dataset | uspto-grants-2003_06 |
| ORD ID | ord-97091d261ab84c56a4b92a9a4c3072e1 |
| Source note | uspto-grants-2003_06 |