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氯化苄 → 4-Benzyloxy-6-methyl-2H-pyran-2-one
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 氯化苄 | HCID 7503 | — |
| 反应物 | 碳酸钾 | HCID 11430 | — |
| 反应物 | 18-冠醚-6 | HCID 28557 | — |
| 反应物 | 4-羟基-6-甲基-2-吡喃酮 | HCID 54675757 | — |
| 溶剂 | N,N-二甲基甲酰胺 | HCID 6228 | — |
| 产物 | 4-Benzyloxy-6-methyl-2H-pyran-2-one | HCID 2784449 | — |
反应步骤
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.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US05731344 |
| 来源数据集 | uspto-grants-1998_03 |
| ORD ID | ord-9faac40bc60f4f9481fb3e21ace77f7b |
| 来源说明 | uspto-grants-1998_03 |