関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-(4-Chlorophenoxy)phenol | HCID 12346120 | — |
| 反応物 | 2-Chloro-1-(isoxazolidin-2-yl)propan-1-one | HCID 13314616 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-[4-(4-Chlorophenoxy)phenoxy]-1-(1,2-oxazolidin-2-yl)propan-1-one | HCID 13314618 | 95.9% |
反応手順
A mixture of 4-(4-chlorophenoxy)phenol (22.1 g), N-[(±)-2-chloropropionyl]isoxazolidine (16.4 g) which was prepared as in Example 1, anhydrous potassium carbonate (15.2 g) and acetonitrile (300 ml) was heated under reflux with stirring for 5 hours. After cooling, the reaction mixture was filtered through a suction filter to remove solid matters and the filtrate was concentrated in vacuo. The residue was washed with the addition of water and benzene and the organic layer formed was separated and dried over anhydrous sodium sulfate. The removal of the solvent by a distillation in vacuo gave N-[(±)-2-[4-(4-chlorophenoxy)phenoxy]propionyl]isoxazolidine (33.4 g) as a pale yellow crystalline solid. Recrystallization from a mixture of n-hexane/ethyl acetate yielded a white crystalline solid. m.p. 98°-100° 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-6ec89ef5bd1346e989863f9155450ad7 |
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| 出典メモ | uspto-grants-1984_05 |
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