Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triphenylphosphine → 2-Bromo-1-((2-chloro-5-(trifluoromethyl)phenoxy)methyl)-3-methylbenzene
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | Phenol, 2-chloro-5-(trifluoromethyl)- | HCID 123498 | — |
| 반응물 | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| 반응물 | (2-Bromo-3-methylphenyl)methanol | HCID 52987706 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2-Bromo-1-((2-chloro-5-(trifluoromethyl)phenoxy)methyl)-3-methylbenzene | HCID 67324702 | — |
반응 단계
To a solution of (2-bromo-3-methylphenyl)methanol (0.5 g, 2.49 mmol), triphenylphosphine (1.31 g, 4.97 mmol) and 2-chloro-5-(trifluoromethyl)phenol (0.37 mL, 2.74 mmol) in DCM (12.4 mL) at 0° C. was added diethyl azodicarboxylate (1.97 mL, 4.97 mmol) and the reaction warmed to RT for 30 min. The reaction was quenched with water and the aqueous layer was extracted with EtOAc. The organic layer was then washed with water and brine (3× ea.), dried over Na2SO4 and concentrated in vacuo. The crude material was purified by column chromatography (0-50% Hexene/EtOAc) to afford 2-bromo-1-((2-chloro-5-(trifluoromethyl)phenoxy)methyl)-3-methylbenzene as a clear oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08735384B2 |
| 출처 데이터셋 | uspto-grants-2014_05 |
| ORD ID | ord-e3f1a608aece4bdfb61e9b6616cbd648 |
| 출처 메모 | uspto-grants-2014_05 |