Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triphenylphosphine → 3-Chloro-5-[2-(4-cyanophenyl)ethoxy]phenol
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | 1,3-Benzenediol, 5-chloro- | HCID 94554 | — |
| 반응물 | 4-(2-Hydroxyethyl)benzonitrile | HCID 2800815 | — |
| 반응물 | Diethyl azodicarboxylate | HCID 5462977 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 3-Chloro-5-[2-(4-cyanophenyl)ethoxy]phenol | HCID 22033534 | 21.3% |
반응 단계
Triphenylphoshine (32 g; 122 mmol) and diethylazodicarboxylate (19.2 mL; 122 mmol) were dissolved in CH2Cl2 (150 mL). Chloro-3,5-dihydroxybenzene (9.1 g; 63 mmol; from step (i) above) and 2-(4-cyanophenyl)ethanol (9.04 g; 61 mmol) were added and the solution was stirred at room temperature overnight. The mixture was diluted with Et2O and filtered through Celite. The solvent was removed in vacuo. Purification, first by flash chromatography (SiO2; CH2Cl2:MeOH), then by preparative HPLC (60% CH3CN:0.1 M NH4OAc/aq), afforded 3.55 g (21%) of the sub-title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06221898B1 |
| 출처 데이터셋 | uspto-grants-2001_04 |
| ORD ID | ord-b142d67c5d7743cc8446130949fd67d9 |
| 출처 메모 | uspto-grants-2001_04 |