関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Neopentyl alcohol | HCID 6404 | — |
| 反応物 | 6-Chloronicotinoyl Chloride | HCID 2782165 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2,2-Dimethylpropyl 6-chloropyridine-3-carboxylate | HCID 86659746 | 92% |
反応手順
To a solution of 10 g (56.8 mmol) of 6-chloropyridine-3-carbonyl chloride in 100 mL of anhydrous toluene are added under argon, at room temperature, 15 g (170.4 mmol) of 2,2-dimethylpropanol. The reaction medium is then heated for 6 hours at 80° C. After cooling to room temperature, the medium is concentrated and the residue obtained is taken up in 800 mL of EtOAc, washed successively with water (2×200 mL), saturated NaHCO3 solution (2×200 mL) and brine (100 mL), dried over Na2SO4, and then concentrated under reduced pressure and purified by chromatography on a column of silica gel, eluting with a cyclohexane/EtOAc gradient of 0 to 5% EtOAc. 11.9 g of 2,2-dimethylpropyl 6-chloropyridine-3-carboxylate are obtained in the form of a white powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08541455B2 |
|---|
| 出典データセット | uspto-grants-2013_09 |
|---|
| ORD ID | ord-095d32159f074af9a6090351ff177e40 |
|---|
| 出典メモ | uspto-grants-2013_09 |
|---|