HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → methyl 2-[1-(N-allyloxyimino)ethyl]-6-[(4,6-dimethoxypyrimidin-2-yl)oxy]benzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Potassium Acetate | HCID 517044 | — |
| Reactant | O-Allylhydroxylamine hydrochloride | HCID 3084724 | — |
| Reactant | HCID 19089394 | HCID 19089394 | — |
| Solvent | Water | HCID 962 | — |
| Product | methyl 2-[1-(N-allyloxyimino)ethyl]-6-[(4,6-dimethoxypyrimidin-2-yl)oxy]benzoate | HCID 85216991 | 46.3% |
Reaction Steps
1.0 g of methyl 2-acetyl-6-[(4,6-dimethoxypyrimidin-2-yl)oxy]benzoate, 1.0 g of allyloxyamine hydrochloride and 0.9 g of potassium acetate were added to 30 ml of methanol, and were refluxed with stirring for 5 hours. The reaction mixture was then poured into a cold water, and was extracted with ethyl acetate. The organic layer thus formed was washed with firstly dilute hydrochloric acid, then sodium hydrogencarbonate and water in sequence. The organic layer thus washed was then dried and concentrated. The residue oily product was purified by column chromatography to obtain 0.54 g of the aimed compound (melting point=76° to 78° C.) at a yield of 46% as a colorless transparent crystal.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05242895 |
| Source dataset | uspto-grants-1993_09 |
| ORD ID | ord-f731ed3622dd4070b9453e090fd140d9 |
| Source note | uspto-grants-1993_09 |