HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 59355290, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 1,2-Dimethylhydrazine dihydrochloride | HCID 9380 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 59355358 | HCID 59355358 | — |
| Catalyst | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 59355290 | HCID 59355290 | 88.3% |
Reaction Steps
1,2-Dimethylhydrazine dihydrochloride (176 mg) and potassium carbonate (366 mg) were suspended in THF (8 mL) and 10 drops of water, 2-[5-bromo-2-(3-chloro-pyridin-2-yl)-2H-pyrazol-3-yl]-6-chloro-8-methyl-pyrido[3,2-d][1,3]oxazin-4-one (example 7, step 4) (300 mg) was added and the reaction mixture was stirred for 20 h at room temperature. Water and ethyl acetate were added, the layers were separated and the aqueous layer was 2× extracted with ethyl acetate. The combined organic layer was washed with brine, dried over magnesium sulfate and concentrated in vacuum. The residue was purified by column chromatography (silica 60, chloroform/ethyl acetate=1:1, Rf=0.13) to afford 300 mg of the title compound of the formula
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08247431B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-13b350d5558047c3a1a785187e60fe31 |
| Source note | uspto-grants-2012_08 |