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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 in 400 ml of acetonitrile with 100 g of potassium carbonate and 32 ml of chloroacetone are stirred under reflux for 30 hours. After the addition of a further 3.2 ml of chloroacetone, the reaction mixture is refluxed for a further 15-20 hours. The reaction mixture is filtered whilst still warm; the residue is 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, m.p. 125°-126°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04497813 |
| 出典データセット | uspto-grants-1985_02 |
| ORD ID | ord-ce006c809b9e4b24a79f84d254d6d71c |
| 出典メモ | uspto-grants-1985_02 |