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Thionyl Chloride → 4-(2-Chloro-4-chloromethylphenoxy)methyl-2-(2-furyl)-5-methyl-1,3-oxazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | (3-Chloro-4-{[2-(2-furyl)-5-methyl-1,3-oxazol-4-yl]methoxy}phenyl)methanol | HCID 23076380 | — |
| 生成物 | 4-(2-Chloro-4-chloromethylphenoxy)methyl-2-(2-furyl)-5-methyl-1,3-oxazole | HCID 23076566 | 94% |
反応手順
(3-Chloro-4-{[2-(2-furyl)-5-methyl-1,3-oxazol-4-yl]methoxy}phenyl)methanol (4.0 g) was added to thionyl chloride (10 mL) at 0° C., and the mixture was stirred for 2 hrs. The reaction mixture was concentrated, saturated aqueous sodium hydrogen carbonate was added to the residue and the mixture was extracted with ethyl acetate. The organic layer was washed successively with saturated aqueous sodium hydrogen carbonate and saturated brine, dried over anhydrous magnesium sulfate and concentrated to give 4-(2-chloro-4-chloromethylphenoxy)methyl-2-(2-furyl)-5-methyl-1,3-oxazole as colorless crystals (3.96 g, yield 94%). Recrystallization from ethyl acetate-hexane gave colorless needle crystals. melting point: 103-104° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07368578B2 |
| 出典データセット | uspto-grants-2008_05 |
| ORD ID | ord-f54b9f553bf447a1b267380a2f57aabf |
| 出典メモ | uspto-grants-2008_05 |