Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2-(Dicyclohexylphosphino)-2'-(dimethylamino)biphenyl → [2,6-Dimethyl-4-(6-trifluoromethyl-3,4-dihydro-1H-isoquinolin-2-yl)-phenyl]-carbamic acid ethyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2-(Dicyclohexylphosphino)-2'-(dimethylamino)biphenyl | HCID 2734217 | — |
| 반응물 | (4-Bromo-2,6-dimethyl-phenyl)-carbamic acid ethyl ester | HCID 11644748 | — |
| 반응물 | 6-(Trifluoromethyl)-1,2,3,4-tetrahydroisoquinoline hydrochloride | HCID 21712558 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | [2,6-Dimethyl-4-(6-trifluoromethyl-3,4-dihydro-1H-isoquinolin-2-yl)-phenyl]-carbamic acid ethyl ester | HCID 58097366 | — |
반응 단계
Bis(dibenzylidineacetone)palladium (17 mg, 0.03 mmol) and (2′-dicyclohexylphosphanyl-biphenyl-2-yl)-dimethylamine (35 mg, 0.09 mmol) were added to dry toluene (5 mL purged with argon) and stirred for 15 minutes under argon. Potassium tert-butoxide (166 mg, 1.48 mmol), 6-Trifluoromethyl-1,2,3,4-tetrahydro-isoquinoline hydrochloride salt (176 mg, 0.74 mmol) and (4-Bromo-2,6-dimethyl-phenyl)-carbamic acid ethyl ester (200 mg, 0.74 mmol) were then added and the reaction mixture was stirred at 80° C. overnight. The reaction mixture was then cooled to room temperature filtered through silica gel and purified by preparative thin layer chromatography (DCM 100%) to give the desired compound as a solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08293911B2 |
| 출처 데이터셋 | uspto-grants-2012_10 |
| ORD ID | ord-be953970d82f45b9bce8a6e4464bb3a0 |
| 출처 메모 | uspto-grants-2012_10 |