関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 反応物 | 1-(2-(Benzyloxy)-4-fluorophenyl)ethanone | HCID 21241577 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(Benzyloxy)-4-fluorophenol | HCID 21241585 | 93% |
反応手順
A mixture of 11 parts of 1-[4-fluoro-2-(phenylmethoxy)phenyl]ethanone, 8.48 parts of 3-chlorobenzenecarboperoxoic acid and 260 parts of dichloromethane was stirred for 5 days at room temperature. The precipitate was filtered off and the filtrate was stirred in a saturate thiosulfate solution for 15 minutes. The organic layer was separated and stirred in a saturate hydrogen carbonate solution for 15 minutes. The organic layer was separated, washed with water, dried, filtered and evaporated. The solid residue was stirred in 240 parts of methanol. 5.3 Parts of sodium methoxide were added portionwise. After complete addition, the whole was stirred for 1 hour at room temperature. After evaporation in vacuo at 50° C., the residue was stirred in water and acidified with a hydrochloric acid solution 3N. Trichloromethane was added, the organic layer was separated, washed twice with water, dried, filtered and evaporated, yielding 10 parts (93%) of 4-fluoro-2-(phenylmethoxy)phenol as a residue (intermediate 77).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04826848 |
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| 出典データセット | uspto-grants-1989_05 |
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| ORD ID | ord-98ef6346155b4b628f441ff4dffa1707 |
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| 出典メモ | uspto-grants-1989_05 |
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