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Dimethylamine → n-[4-(6-Chloro-3,4-dihydro-1h-isoquinolin-2-yl)-2,6-dimethyl-phenyl]-3,3-dimethylbutanamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylamine | HCID 674 | — |
| 反応物 | 6-Chloro-1,2,3,4-Tetrahydroisoquinoline Hydrochloride | HCID 12595084 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 反応物 | N-(4-Bromo-2,6-dimethyl-phenyl)-3,3-dimethyl-butanamide | HCID 59741059 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | n-[4-(6-Chloro-3,4-dihydro-1h-isoquinolin-2-yl)-2,6-dimethyl-phenyl]-3,3-dimethylbutanamide | HCID 24937081 | — |
反応手順
Bis(dibenzylidineacetone)palladium (2 mg, 0.0035 mmol) and 2′-dicyclohexylphosphanyl-biphenyl-2-yl)-dimethylamine (3.3 mg, 0.0084 mmol) were added to dry toluene (5 mL purged with argon) and stirred for 15 minutes under argon. Potassium tert-butoxide (188 mg, 1.7 mmol), 6-chloro-1,2,3,4-tetrahydro isoquinoline hydrochloride salt (165 mg, 0.8 mmol), and N-(4-bromo-2,6-dimethylphenyl)-3,3-dimethylbutanamide (200 mg, 0.67 mmol) were then added, and the reaction mixture was stirred at 80° C. overnight. The reaction mixture was then cooled to room temperature and filtered through silica gel. Purification by preparative thin layer chromatography afforded the title compound as a solid.
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-acc41914cd3f4b08bc453d2c44301d73 |
| 出典メモ | uspto-grants-2015_03 |