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Potassium tert-butoxide → 4-(6-Fluoro-3,4-dihydro-1H-isoquinolin-2-yl)-2,6-dimethylphenyl-3,3-dimethyl butanamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 反応物 | 6-Fluoro-1,2,3,4-tetrahydroisoquinoline hydrochloride | HCID 45074042 | — |
| 反応物 | N-(4-Bromo-2,6-dimethyl-phenyl)-3,3-dimethyl-butanamide | HCID 59741059 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-(6-Fluoro-3,4-dihydro-1H-isoquinolin-2-yl)-2,6-dimethylphenyl-3,3-dimethyl butanamide | HCID 86649628 | — |
反応手順
Bis(dibenzylidineacetone)palladium (390 mg, 0.68 mmol) and (2′-dicyclohexyl phosphanyl-biphenyl-2-yl)-dimethylamine (800 mg, 2.0 mmol) were added to dry toluene (150 mL purged with argon for 30 minutes) and stirred for 30 minutes under argon. Potassium tert-butoxide (4.75 mg, 42.3 mmol), 6-fluoro-1,2,3,4-tetrahydro-isoquinoline hydrochloride salt (3.2 g, 17.0 mmol), and N-(4-bromo-2,6-dimethyl-phenyl)-3,3-dimethyl-butanamide (5 g, 16.8 mmol) were then added, and the reaction mixture was stirred at 80° C. overnight. The reaction mixture was then cooled to room temperature and recrystallized from toluene to afford the title compound as a solid. (5.11 g, 83%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08993593B2 |
| 出典データセット | uspto-grants-2015_03 |
| ORD ID | ord-2465b035f16a400ebdefc9548d845fee |
| 出典メモ | uspto-grants-2015_03 |