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Butanedione → 6-cyano-3,4-dihydro-2,2-dimethyl-4-(2,5-dimethyl-3-furyl)-2H-1,4-benzoxazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Butanedione | HCID 650 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 6-cyano-3,4-dihydro-2,2-dimethyl-2H-1,4-benzoxazine | HCID 10535622 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 6-cyano-3,4-dihydro-2,2-dimethyl-4-(2,5-dimethyl-3-furyl)-2H-1,4-benzoxazine | HCID 19934572 | — |
反応手順
In 2 ml of toluene were dissolved 0.5 g of 6-cyano3,4-dihydro-2,2-dimethyl-2H-1,4-benzoxazine, 1.2 ml of 2,3-butanedione and a catalytic amount of p-toluenesulfonic acid and the mixture was stirred at 100° C. for 2 days. The solvent was then distilled off under reduced pressure and the residue was re-dissolved in toluene, washed with saturated aqueous sodium hydrogen carbonate solution and saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate. The solvent was then distilled off and the residue was purified by silica gel column chromatography to give 0.15 g of 6-cyano-3,4-dihydro-2,2-dimethyl-4-(2,5-dimethyl-3-furyl)-2H-1,4-benzoxazine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05420126 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-1cb012ca07d148ccb63022c8e5fbaf45 |
| 出典メモ | uspto-grants-1995_05 |