Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triphenylphosphine → 1-(3-Bromo-4-{[(4-chloro-2-pyridinyl)methyl]oxy}phenyl)ethanone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | 1-(3-Bromo-4-hydroxyphenyl)ethanone | HCID 608094 | — |
| 반응물 | (4-Chloropyridin-2-yl)methanol | HCID 2763167 | — |
| 반응물 | Diethyl azodicarboxylate | HCID 5462977 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-(3-Bromo-4-{[(4-chloro-2-pyridinyl)methyl]oxy}phenyl)ethanone | HCID 68201960 | — |
반응 단계
To a stirred solution of (4-chloro-2-pyridinyl)methanol (Commercial eg Aldrich) (0.2 g) in THF (5 ml) were added 1-(3-bromo-4-hydroxyphenyl)ethanone (0.3 g) and triphenylphosphine (0.547 g). This was stirred for 10 min before cooling and adding slowly DEAD (0.363 g). This was stirred for 16 h. The reaction mixture was partitioned between water and ethyl acetate. The aqueous was reextracted with ethyl acetate and the combined organics were washed with brine, dried over sodium sulfate and concentrated in vacuo. This was purified through silica eluting with 0-35% ethyl acetate in hexane to give the title compound, 0.30 g
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09447074B2 |
| 출처 데이터셋 | uspto-grants-2016_09 |
| ORD ID | ord-a429b1da3344417d94b8f0ecf4efed2d |
| 출처 메모 | uspto-grants-2016_09 |