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Water → Fluorenone-2-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Sodium Dichromate | HCID 25408 | — |
| 反応物 | 2-Acetylfluorene | HCID 69908 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | Fluorenone-2-carboxylic acid | HCID 69913 | — |
反応手順
A solution of 2-acetylfluorene (86 g.) in acetic acid (1075 ml.) at 60° was treated slowly with sodium dichromate (1020 g.), and then with acetic anhydride (285 ml.). The mixture was heated to reflux with stirring for 3 hours, cooled and poured into water (6 l.), and the precipitate was filtered and washed well with water. This solid was warmed with N-sodium hydroxide (520 ml.) and the mixture was filtered. The aqueous filtrate was washed three times with dichloromethane (3 × 60 ml.) and then heated on the steam-bath and cautiously acidified with hydrochloric acid. The yellow product was filtered, washed well with water and dried in vacuo to give fluorenone-2-carboxylic acid m.p. > 300°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03939276 |
| 出典データセット | uspto-grants-1976_02 |
| ORD ID | ord-061406e8a0714d5bae742189b8e80d81 |
| 出典メモ | uspto-grants-1976_02 |