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tert-Butanol → tert-Butyl (2-cyanopyridin-4-yl)carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | tert-Butanol | HCID 6386 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| 反応物 | 2-Cyanoisonicotinic Acid | HCID 2762513 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | tert-Butyl (2-cyanopyridin-4-yl)carbamate | HCID 22939607 | — |
反応手順
While stirring at room temperature, 1.8 ml of triethylamine and 2.8 ml of DPPA were added in that order to 100 ml of t-butanol solution containing 1.5 g of 2-cyanoisonicotinic acid, and the mixture was heated under refulx for 4 hours and 25 minutes. The reaction mixture was cooled to room temperature, mixed with water and extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium bicarbonate and dried over anhydrous sodium sulfate, and then the solvent was evaporated under reduced pressure. The residue was purified by a silica gel column chromatography, and 1.34 g of the title compound was obtained from ethyl acetate-hexane (1:2, v/v) eluate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06673799B1 |
| 出典データセット | uspto-grants-2004_01 |
| ORD ID | ord-d792eb831adb4ae8936f7104c890d60a |
| 出典メモ | uspto-grants-2004_01 |