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Phenacyl bromide → 4-[3-(4,5-Dihydroisoxazol-3-yl)-4-methylsulfonyl-2-methylbenzoyl]-1-ethyl-5-phenacyloxypyrazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phenacyl bromide | HCID 6259 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | HCID 178463114 | HCID 178463114 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-[3-(4,5-Dihydroisoxazol-3-yl)-4-methylsulfonyl-2-methylbenzoyl]-1-ethyl-5-phenacyloxypyrazole | HCID 15477457 | 64.7% |
反応手順
0.20 g of 4-[3-(4,5-dihydroisoxazol-3-yl)-4-methylsulfonyl-2-methylbenzoyl]-1-ethyl-5-hydroxypyrazole was dissolved in 10 ml of DMF, and 0.11 g of potassium carbonate, then 0.13 g of phenacyl bromide were added. The resulting solution was stirred at room temperature overnight. The reaction solution was poured into ice water, and extracted with ethyl acetate. The organic layer was washed with water, then with a saturated sodium chloride solution, and dried over anhydrous magnesium sulfate. The solvent was distilled out under reduced pressure. Methanol was added to the residue. The obtained crystals were separated by filtration to give 0.17 g of the title compound as white crystals. m.p. 177~179° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06147031 |
| 出典データセット | uspto-grants-2000_11 |
| ORD ID | ord-abb9c3034bb7408e91264ea05b3bd8b6 |
| 出典メモ | uspto-grants-2000_11 |