Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Potassium Fluoride → Methyl [3,5-bis(trifluoromethyl)benzyl]{[2'-cyano-4-(trifluoromethyl)biphenyl-2-yl]methyl}carbamate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Potassium Fluoride | HCID 522689 | — |
| 반응물 | 2-(Dicyclohexylphosphino)biphenyl | HCID 2734216 | — |
| 반응물 | 2-Cyanophenylboronic acid | HCID 2734610 | — |
| 반응물 | Methyl [3,5-bis(trifluoromethyl)benzyl](2-iodo-5-trifluoromethyl-benzyl)carbamate | HCID 59343876 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | Methyl [3,5-bis(trifluoromethyl)benzyl]{[2'-cyano-4-(trifluoromethyl)biphenyl-2-yl]methyl}carbamate | HCID 11577673 | — |
반응 단계
A mixture of methyl [3,5-bis(trifluoromethyl)benzyl](2-iodo-5-trifluoromethyl-benzyl)carbamate (29 mg, 0.050 mmol), 2-cyanophenylboronic acid (10.9 mg, 0.074 mmol), potassium fluoride (8.7 mg, 0.149 mmol), 2-dicyclohexylphosphino(biphenyl) ligand (0.7 mg, 0.002 mmol) and a catalytic amount of palladium acetate was stirred in dioxane overnight at 80° C. The title compound was obtained by preparative thin layer chromatography using 20% EtOAc/hexane. 1H NMR (CDCl3, 600 MHz) δ 7.74 (m, 2H), 7.68 (d, J=7.8 Hz, 1H), 7.64 (t, J=7.8 Hz, 1H), 7.58 (t, J=7.8 Hz, 1H), 7.52 (m, 3H), 7.39 (d, J=7.2 Hz, 1H), 7.24 (m, 1H), 4.30-4.55 (m, 4H), 3.71 (s, 3H). LC-MS (M+1) 561.0 (4.29 min).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08193365B2 |
| 출처 데이터셋 | uspto-grants-2012_06 |
| ORD ID | ord-fec822e574c74f6088d2d3f14312f763 |
| 출처 메모 | uspto-grants-2012_06 |