関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetone Cyanohydrin | HCID 6406 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | HCID 22129431 | HCID 22129431 | — |
| 反応物 | HCID 178463041 | HCID 178463041 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | HCID 178463113 | HCID 178463113 | — |
反応手順
Separately 0.38 g of 1-ethyl-5-hydroxypyrazole hydrochloride was dissolved in 10 ml of chloroform, and 0.52 g of triethylamine was added, while cooling with ice. Into the obtained solution was added dropwise 5 ml of a chloroform solution containing the previously obtained 3-(isoxazol-3-yl)-4-methylsulfonyl-2-methylbenzoyl chloride to stir at room temperature for an hour. To the reaction mixture were added 0.26 g of triethylamine and 0.05 g of acetone cyanohydrin to further stir overnight. The reaction solution was washed with dilute hydrochloric acid, 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 obtained residue. The produced crystals were separated by filtration to give 0.18 g of the title compound as white crystals. m.p. 85~88° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06147031 |
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| 出典データセット | uspto-grants-2000_11 |
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| ORD ID | ord-243ab9a9659348e398e39911fd9e8f5c |
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| 出典メモ | uspto-grants-2000_11 |
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