Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylformamide → [3-(4-{1-[4-(4-Chloro-phenoxy)-phenyl]-2-isobutyl-1h-imidazol-4-yl}-phenoxy)-propyl]-diethyl-amine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | 4-(4-Chlorophenoxy)aniline | HCID 7578 | — |
| 반응물 | 2-Bromo-1-{4-[3-(diethylamino)propoxy]phenyl}ethanone | HCID 86591969 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | [3-(4-{1-[4-(4-Chloro-phenoxy)-phenyl]-2-isobutyl-1h-imidazol-4-yl}-phenoxy)-propyl]-diethyl-amine | HCID 25144973 | — |
반응 단계
To a stirred solution of 4-amino-4′-chlorodiphenyl ether (1.2 eq., 6.2 mmol) in anhydrous DMF (10 mL) DIEA (3 eq. 16 mmol) was added, followed by slow addition of the 2-bromo-1-{4-[3-(diethylamino)propoxy]phenyl}ethanone described above (5.2 mmol), according to General Procedure R2. The reaction mixture was stirred under nitrogen at rt until completion, as indicated by TLC or HPLC. The reaction mixture was then diluted with cold H2O and the product was extracted in EtOAc. The combined organic layers were washed with brine and dried over sodium sulfate. Evaporation of solvent in vacuuo afforded the desired product. The crude alkylated aniline was purified by chromatography (Silica gel). Pure product obtained from 2-4% MeOH/DCM (yield˜22%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07737285B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-dbc193f488134261901b8ecf05a8a207 |
| 출처 메모 | uspto-grants-2010_06 |