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Salicylamide → 2,2-dibutyl-4-oxo-2,3-dihydro-4H-1,3-benzoxazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Salicylamide | HCID 5147 | — |
| 反応物 | 5-Nonanone | HCID 10405 | — |
| 反応物 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2,2-dibutyl-4-oxo-2,3-dihydro-4H-1,3-benzoxazine | HCID 10084017 | 92.5% |
反応手順
A mixture of 20 g of dibutylketone, 19.3 g of salicylamide and 2.7 g of p-toluenesulfonic acid monohydrate is added to 300 ml of toluene and the mixture is refluxed overnight by making use of a dehydrator of Dean Stark. After cooling, the reaction mixture is washed, dried and evaporated to remove the solvent. The residue is purified by silica gel column chromatography (solvent; hexane:ethyl acetate=95:5) to obtain 34 g of 2,2-dibutyl-4-oxo-2,3-dihydro-4H-1,3-benzoxazine as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06011150 |
| 出典データセット | uspto-grants-2000_01 |
| ORD ID | ord-c6d2c609d24a44d1bf46a6f36adbfdfb |
| 出典メモ | uspto-grants-2000_01 |