関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| 反応物 | 5-(Benzyloxy)-2-chloropyridine | HCID 10013717 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-Benzyloxy-pyridin-2-ylamine hydrochloride | HCID 66995170 | 98.94% |
反応手順
To a nitrogen purged solution of mL Pd2 (dba)3 (10.19 g, 11.12 mmol), 5-(benzyloxy)-2-chloropyridine (48.87 g, 222.5 mmol), (2-diphenyl)dicyclohexyl-phosphine (7.797 g, 22.25 mmol) and THF (700 mL) was added lithium hexamethyl disilazide (267.0 mL, 267.0 mmol). The reaction was heated at 65° C. overnight and cooled to ambient temperature. 1M HCl (250 mL) was added and stirred for minutes. Saturated sodium bicarbonate was added slowly. The mixture was extracted several times with CH2Cl2, dried, filtered, and concentrated to give the title compound (52.1 g, 98.94% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08883828B2 |
|---|
| 出典データセット | uspto-grants-2014_11 |
|---|
| ORD ID | ord-df42bb9ffab44f3180050693d20fa6f0 |
|---|
| 出典メモ | uspto-grants-2014_11 |
|---|
