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Dichloroacetyl chloride → Benoxacor
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloroacetyl chloride | HCID 6593 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 3-Methyl-3,4-dihydro-2H-1,4-benzoxazine | HCID 2763760 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | Benoxacor | HCID 62306 | 83% |
反応手順
5.3 ml (55 mmoles) of dichloroacetyl chloride are added dropwise, at a temperature of 20° to 25° C. and while stirring, to a suspension of 7.5 g (50 mmoles) of 2,3-dihydro-3-methyl-1,4-benzoxazine and 5.8 g (55 mmoles) of sodium carbonate in 120 ml of benzene. The reaction mixture is then stirred at the same temperature for 30 minutes and is then taken up in a mixture of water and ethyl acetate. The organic phase is washed with saturated sodium chloride solution, dried over sodium sulfate and evaporated. Crystallising the residue from diisopropyl ether gives 10.8 g of 4-dichloroacetyl-2,3-dihydro-3-methyl-1,4-benzoxazine, melting point 105°-107° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04618361 |
| 出典データセット | uspto-grants-1986_10 |
| ORD ID | ord-e9aaa438dd1e4caf875d550daa2465a4 |
| 出典メモ | uspto-grants-1986_10 |