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Sulfuric Acid → 4-(Chloromethyl)-2-(3,4-difluorophenyl)-1,3-oxazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 1,3-Dichloroacetone | HCID 10793 | — |
| 反応物 | 3,4-Difluorobenzamide | HCID 522832 | — |
| 生成物 | 4-(Chloromethyl)-2-(3,4-difluorophenyl)-1,3-oxazole | HCID 50989423 | — |
反応手順
With stirring, 500 mg (3.94 mmol) of 1,3-dichloroacetone and 619 mg (3.94 mmol) of 3,4-difluorobenzamide are heated at +135° C. for 1 h. After cooling to RT, the mixture is allowed to stand at this temperature for 90 min 1.0 ml of conc. sulphuric acid is then added, and the mixture is stirred at RT for a further 15 min. The entire mixture is then poured onto 50 ml of ice. Initially, a viscous oil is formed. The mixture is stirred for 60 min, during which time a precipitate is formed which is filtered off with suction, dried under high vacuum and then purified chromatographically on silica gel 60 (mobile phase: isohexane/ethyl acetate 10:1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08653109B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-282074a588984a62bfbcf31747bfaa56 |
| 出典メモ | uspto-grants-2014_02 |