関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Borane;tetrahydrofuran | HCID 2723981 | — |
| 反応物 | 2-(Methylthio)picolinic acid | HCID 22018528 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | [2-(Methylsulfanyl)pyridin-3-yl]methanol | HCID 22018843 | 30.3% |
反応手順
To 2-(methylthio)picolinic acid (1.00 g, 5.91 mmol) was added BH3.THF (1.0 M/THF, 15 mL, 15 mmol) and the mixture heated at 80° C. for 24 h. Methanol (30 mL) was carefully added at room temperature and the solution was concentrated in vacuo. Purification of the crude material on silica gel (20% EtOAc/hexanes) gave the title compound as colourless crystals (278 mg, 30%). 1H NMR (CDCl3) □ 1.99 (t, 1H, J=6.0 Hz), 2.61 (s, 3H), 4.70 (d, 2H, J=6.0 Hz), 7.04 (dd, 1H, J=6, 3 Hz), 7.62 (d, 1H, J=6 Hz), 8.40 (d, 1H, J=3 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07084155B2 |
|---|
| 出典データセット | uspto-grants-2006_08 |
|---|
| ORD ID | ord-8ca8621f578e448293bc81423498fb78 |
|---|
| 出典メモ | uspto-grants-2006_08 |
|---|