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Chloroacetone → 2,3-dihydro-2,2-dimethyl-6-(2-oxopropoxy)-4H-1,3-benzoxazin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroacetone | HCID 6571 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 6-hydroxy-2,2-dimethyl-3,4-dihydro-2H-1,3-benzoxazin-4-one | HCID 13754331 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2,3-dihydro-2,2-dimethyl-6-(2-oxopropoxy)-4H-1,3-benzoxazin-4-one | HCID 13754332 | — |
反応手順
70 g of 2,3-dihydro-2,2-dimethyl-6-hydroxy-4H-1,3-benzoxazin-4-one are refluxed for 30 hours, whilst stirring, in 400 ml of acetonitrile with 100 g of potassium carbonate and 32 ml of chloroacetone. After the addition of a further 3.2 ml of chloroacetone, the reaction mixture is heated for a further 15 to 20 hours. The still warm reaction mixture is filtered, the residue thoroughly washed with acetone and the combined filtrate is concentrated by evaporation. The crystalline residue is recrystallised from toluene and yields 2,3-dihydro-2,2-dimethyl-6-(2-oxopropoxy)-4H-1,3-benzoxazin-4-one having a melting point of 125°-126°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04727067 |
| 出典データセット | uspto-grants-1988_02 |
| ORD ID | ord-469f9aa04d4a4ee282aa8435ec72848a |
| 出典メモ | uspto-grants-1988_02 |