関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Dezinamide | HCID 146291 | — |
| 生成物 | N-Hydroxymethyl-3-[3-(trifluoromethyl)phenoxy]-1-azetidinecarboxamide | HCID 13476972 | 30.5% |
反応手順
A mixture of 0.639 g (0.0024 mole) of 3-[3-(trifluoromethyl)phenoxy]-1-azetidinecarboxamide and 6 ml of 37% formaldehyde solution were heated on a water bath at 65° C. for 1 hr, at which time dissolution was complete. The solution was stirred at room temperature for approximately 60 hr. The reaction mixture was divided into two 15 ml centrifuge tubes each extracted three times with ether. The combined extracts were dried over magnesium sulfate, decolorized with charcoal and evaporated to dryness. The residue weighing about 1.5 g was dissolved in ether, washed 5 times with 3 ml of water each time. The ether layer was again dried over magnesium sulfate and evaporated to dryness. The residue was triturated with hexane and ether to give 0.213 g (30.5%) of white powder, m.p. 113°-115° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04505907 |
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| 出典データセット | uspto-grants-1985_03 |
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| ORD ID | ord-18306cb0530b4e47bf7341870223ce28 |
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| 出典メモ | uspto-grants-1985_03 |
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