関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | (+)-Benzylphenethylamine | HCID 1268086 | — |
| 反応物 | 3-(6-Amino-pyridin-3-yl)-acrylic acid tert-butyl ester | HCID 53665462 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 70234416 | HCID 70234416 | — |
反応手順
To a cooled (0° C.) solution of (R)-(+)-N-benzyl-α-methylbenzylamine (4.0 g, 19 mmol) in 50 mL THF was gradually added n-butyllithium (11.3 mL, 2.5 M, 28.2 mmol) over 5 min. The mixture was stirred for 30 min at 0° C. and cooled to -78° C. A solution of 9-2 (2.0 g, 9.4 mmol) in 20 mL THF was gradually added. After stirring for 40 min at -78° C., it was treated with NH4Cl (sat.) at -78° C., warmed to room temperature and extracted three times with EtOAc. The combined organic layers were washed with brine and dried over Na2SO4. After solvent evaporation, the residue was purified using silica gel flash chromatography (EtOAc/hexanes, 1:2) to afford the desired product 9-3 as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06017926 |
|---|
| 出典データセット | uspto-grants-2000_01 |
|---|
| ORD ID | ord-a3a1a044c4b7454fab5ee1e58e0d02ce |
|---|
| 出典メモ | uspto-grants-2000_01 |
|---|