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Benzyl Chloride → 4-Benzyloxy-6-methyl-2H-pyran-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzyl Chloride | HCID 7503 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 18-Crown-6 | HCID 28557 | — |
| 反応物 | 4-Hydroxy-6-methyl-2-pyrone | HCID 54675757 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-Benzyloxy-6-methyl-2H-pyran-2-one | HCID 2784449 | — |
反応手順
124.4 g (0.900 mol) potassium carbonate and 63 ml (0.547 mol) benzyl chloride were added in succession to a solution of 56.7 g (0.450 mol) 4-hydroxy-6-methyl-2H-pyran-2-one and 1.0 g (0.004 mol) 18-crown-6 in 900 ml anhydrous dimethyl-formamide. It was stirred vigorously for 4.5 hours at an internal temperature of 70°-75° C. It was suction filtered and the residue was washed well with ethyl acetate. The combined filtrates were extensively evaporated in a vacuum and subsequently poured onto ice water. The aspirated precipitate was recrystallized from t-butylmethyl ether after drying. 69.0 g (71%) V, melting point 92°-93° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05731344 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-9faac40bc60f4f9481fb3e21ace77f7b |
| 出典メモ | uspto-grants-1998_03 |