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Potassium Carbonate → 3-(4-Fluorophenoxy)-N-(2-propynyl)-1-azetidinecarboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Propargylamine | HCID 239041 | — |
| 反応物 | 3-(4-Fluorophenoxy)-1-azetidinecarbonyl chloride | HCID 15053367 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-(4-Fluorophenoxy)-N-(2-propynyl)-1-azetidinecarboxamide | HCID 15053440 | 174.6% |
反応手順
A mixture of 5.52 g (0.022 mole) of crude 3-(4-fluorophenoxy)-1-azetidine carbonyl chloride and 3 g (0.02 mole) of potassium carbonate in 30 ml of tetrahydrofuran was cooled in an ice bath and while stirring treated with 1.1 g (0.02 mole) of propargylamine added dropwise. After stirring for 5 hr, the reaction mixture was diluted with 250 ml of water and the resulting solid collected by filtration to yield 8.67 g of wet product. Recrystallization from acetone after filtration to remove some amorphous material, gave a tacky solid. A second recrystallization from benzene after treating with charcoal yielded 2.7 g (50%) of beige crystals, m.p. 106°-108° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05068231 |
| 出典データセット | uspto-grants-1991_11 |
| ORD ID | ord-eb98af51b55a48c283d1271594879eaa |
| 出典メモ | uspto-grants-1991_11 |