関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Isoxazolidine hydrochloride | HCID 12304500 | — |
| 反応物 | 2-{4-[4-(Trifluoromethyl)phenoxy]phenoxy}propanoyl chloride | HCID 12906015 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(1,2-Oxazolidin-2-yl)-2-{4-[4-(trifluoromethyl)phenoxy]phenoxy}propan-1-one | HCID 13279436 | 97.7% |
反応手順
To a mixture of isoxazolidine hydrochloride (11.0 g) and chloroform (200 ml), under stirring and ice-cooling, was added (±)-2-[4-(4-trifluoromethylphenoxy)phenoxy]propionyl chloride (34.5 g) and then added dropwise triethylamine (22.2 g). After the completion of addition, the reaction mixture was stirred for further 30 minutes at room temperature, to which water was added to form two layers. The organic layer so separated was washed with 1 N hydrochloric acid and then with 1 N aqueous sodium hydroxide and dried over anhydrous sodium sulfate. Removal of the solvent by a distillation in vacuo gave N-[(±)-2-[4-(4-trifluoromethylphenoxy)phenoxy]propionyl]isoxazolidine (37.3 g) as a white crystalline solid. After recrystallization from a mixture of n-hexane/acetone, the resulting white crystalline solid showed the melting point of 105°-107° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04447259 |
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| 出典データセット | uspto-grants-1984_05 |
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| ORD ID | ord-a8959e1479f54b079121103f4d2ac70f |
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| 出典メモ | uspto-grants-1984_05 |
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