참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| 반응물 | 5-(Benzyloxy)-2-chloropyridine | HCID 10013717 | — |
| 촉매 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 5-Benzyloxy-pyridin-2-ylamine hydrochloride | HCID 66995170 | 98.94% |
반응 단계
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).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08883828B2 |
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| 출처 데이터셋 | uspto-grants-2014_11 |
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| ORD ID | ord-df42bb9ffab44f3180050693d20fa6f0 |
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| 출처 메모 | uspto-grants-2014_11 |
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