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Calcium Fluoride → Methyl 4-(fluoromethyl)benzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Calcium Fluoride | HCID 84512 | — |
| 反応物 | Methyl 4-(bromomethyl)benzoate | HCID 256687 | — |
| 反応物 | Potassium Fluoride | HCID 522689 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Methyl 4-(fluoromethyl)benzoate | HCID 21866613 | 78.7% |
反応手順
Dry acetonitrile (150 ml) was added to 25.00 g of methyl 4-(bromomethyl)benzoate, 19.02 g of potassium fluoride and 9.51 g of calcium fluoride, and the mixture was heated to reflux for 3 days. The reaction solution was concentrated. After addition of 200 ml of acetonitrile, insolubles were removed by filtration, and the filtrate was concentrated again. The residue was purified by silica gel column chromatography (YMC•GEL® SIL-60-230/70, n-hexane:ethyl acetate=10:1–4:1), followed by distillation under reduced pressure to provide 14.45 g of the objective compound as colorless oil. B.p. 118.5–119° C./18 mmHg.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06998412B2 |
| 出典データセット | uspto-grants-2006_02 |
| ORD ID | ord-da8c24c5b365428ca729435422979881 |
| 出典メモ | uspto-grants-2006_02 |