2-Fluorothiophenol → 5-(2-Fluorophenylthio)furan-3-carboxylic Acid
反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[SH:8].Br[C:10]1[O:14][CH:13]=[C:12]([C:15]([OH:17])=[O:16])[CH:11]=1>>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[S:8][C:10]1[O:14][CH:13]=[C:12]([C:15]([OH:17])=[O:16])[CH:11]=1参加物
3
実験手順
Following the procedure of Example 13, o-fluorothiophenol (4.02 g., 31.4 mmoles) was reacted with 5-bromofuran-3-carboxylic acid. Isolation according to the procedure of Example 16 gave crude product as an oil. The product was chromatographed on silica gel with ethyl acetate-1/hexane-5/5% acetic acid as eluant. Combination of clean middle cuts, evaporation to dryness and recrystallization from methanol/water gave purified 5-(2-fluorophenylthio)furan-3-carboxylic acid (266 mg., m.p. 100°-103° C., m/e 238).
後処理
- customgave crude product as an oil
- customThe product was chromatographed on silica gel with ethyl acetate-1/hexane-5/5% acetic acid as eluant
- customCombination of clean middle cuts, evaporation
- customto dryness and recrystallization from methanol/water
- customgave
- custompurified 5-(2-fluorophenylthio)furan-3-carboxylic acid (266 mg., m.p. 100°-103° C., m/e 238)
出典と根拠
- ORDレコード
- ord-61a83ef0a6794ef7b4a4aeba74f8d9f4
- 出典データセット
- uspto-grants-1981_08
- 特許番号
- US04282246
反応ノート
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