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Methanol → methyl 2-[1-(N-allyloxyimino)ethyl]-6-[(4,6-dimethoxypyrimidin-2-yl)oxy]benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Potassium Acetate | HCID 517044 | — |
| 反応物 | O-Allylhydroxylamine hydrochloride | HCID 3084724 | — |
| 反応物 | HCID 19089394 | HCID 19089394 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | methyl 2-[1-(N-allyloxyimino)ethyl]-6-[(4,6-dimethoxypyrimidin-2-yl)oxy]benzoate | HCID 85216991 | 46.3% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05242895 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-f731ed3622dd4070b9453e090fd140d9 |
| 出典メモ | uspto-grants-1993_09 |