関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Chloronicotinic acid | HCID 76258 | — |
| 反応物 | 3-Azetidinol, 1-cyclohexyl- | HCID 98585 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Sodium 2-[(1-Cyclohexyl-3-azetidinyl)oxy]-3-pyridine carboxylate | HCID 23696211 | 86% |
反応手順
A solution of 105 g (0.68 mole) of 1-cyclohexyl-3-azetidinol and 106 g (0.68 mole) of 2-chloronicotinic acid in 400 ml of dry dimethylformamide was added at a rapid drop to 52 g (1.35 mole) of 60% sodium hydride/mineral oil suspended in 400 ml of dry dimethylformamide at 60° C. Mild exothermic reaction was noted. After stirring for 2 hr at 60° C., the mixture was filtered. The filter cake was washed with ethylacetate and dried at 80° C./2 mm to give 174 g (86%) of crude title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04727152 |
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| 出典データセット | uspto-grants-1988_02 |
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| ORD ID | ord-a745416737d6407f8a23a934d3424d3d |
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| 出典メモ | uspto-grants-1988_02 |
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