참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Diethylamine | HCID 8021 | — |
| 반응물 | 4-(Bromomethyl)-3-chlorobenzonitrile | HCID 13042093 | — |
| 반응물 | 4-(2-((tert-Butyldimethylsilyl)oxy)ethyl)-1-trityl-1H-imidazole | HCID 66885359 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | Benzonitrile, m-chloro- | HCID 13015 | — |
반응 단계
4-[2-(tert-Butyldimethylsilanyloxy)ethyl]-1-trityl-1H-imidazole (3.98 g, 8.5 mmol) and 4-bromomethyl-3-chlorobenzonitrile (2.93 g, 12.7 mmol) are dissolved in MeCN (40 mL) and heated at 80° C. for 5 h. After cooling to room temperature MeOH (40 mL) and Et2NH (7 mL) are then added and the solution is warmed 70° C. for 1 h. The solution is evaporated to dryness and the residue purified via flash column chromatography (acetone/CH2Cl2 1:3→MeOH/CH2Cl2 5:95) to give 4-{5-[2-tert-butyl-dimethylsilanyloxy)ethyl]-imidazol-1-ylmethyl}-3-chlorobenzonitrile as an oil. MS (ESI) m/z 376.3, 378.3 (M+H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08835646B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_09 |
|---|
| ORD ID | ord-79cdbd8def654cd999b2d85bcce979ca |
|---|
| 출처 메모 | uspto-grants-2014_09 |
|---|
