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Tert-Butylamine → HCID 66661120、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tert-Butylamine | HCID 6385 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Propylphosphonic anhydride | HCID 111923 | — |
| 反応物 | 4-Methylpyridine-2-carboxylic acid | HCID 2762820 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 66661120 | HCID 66661120 | 53.6% |
反応手順
4-Methylpyridine-2-carboxylic acid (500 mg, 3.65 mmol), triethylamine (1.27 g, 12.5 mmol, 1.75 mL) and tert-butylamine (267 mg, 3.65 mmol) were combined and stirred in dichloromethane (1 mL). 1-Propanephosphonic acid cyclic anhydride (4.82 g, 7.5 mmol, 4.5 mL, 50% solution in ethyl acetate) was added dropwise and the reaction stirred at room temperature for 1 hour. The reaction mixture was concentrated at reduced pressure and the resulting residue taken up in ethyl acetate and washed with saturated sodium bicarbonate solution. The organic phase was dried over sodium sulfate and concentrated under vacuum to afford the title compound (376 mg). MS (ESI) m/z 193.4 [M+H]+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08759352B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-56b48c9a327b4901b2f453bf902d264d |
| 出典メモ | uspto-grants-2014_06 |