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Water → 3-Methyl-7-[4-(4-chlorobenzoyl)benzyl]xanthine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Methylxanthine | HCID 70639 | — |
| 反応物 | 4-(4-Chlorobenzoyl)benzyl bromide | HCID 9839651 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-Methyl-7-[4-(4-chlorobenzoyl)benzyl]xanthine | HCID 18918801 | 10% |
反応手順
To a solution of 3-methylxanthine (1.06 g) in DMF (26 ml) were added potassium carbonate (1.06 g) and 4-(4-chlorobenzoyl)benzyl bromide (1.98 g) and the mixture was stirred at room temperature for 24 hours. To this reaction mixture were added water and ethyl acetate and the floating matter was filtered off and the filtrate aqueous solution was diluted with 1N-hydrochloric acid and extracted with chloroform. The extract was washed with saturated aqueous NaCl solution and dried over anhydrous sodium sulfate. The solvent was then distilled off and the residue was washed with ethyl acetate to provide the title compound as colorless powder (239 mg, 10%). 1H-NMR (CDC13) 8: 3.54(3H,s), 3.57(3H,s), 7.41-7.52(4H,m), 7.68-7.81(5H,m).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05753664 |
| 出典データセット | uspto-grants-1998_05 |
| ORD ID | ord-263f4060c9a346398982594f4c89d517 |
| 出典メモ | uspto-grants-1998_05 |