참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 3-Ethoxy-1-propanol | HCID 8109 | — |
| 반응물 | Triphenylphosphine | HCID 11776 | — |
| 반응물 | 4-Bromo-3-chlorophenol | HCID 7018182 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 4-Bromo-3-chloro-(3-ethoxypropoxy)benzene | HCID 21995744 | 79.1% |
반응 단계
To a solution of 4-bromo-3-chlorophenol (10.0 g), 3-ethoxypropanol (6.0 g) and triphenylphosphine (15.2 g) in tetrahydrofuran (50 ml) was added dropwise under nitrogen atmosphere at 0° C. diethylazodicarbonate (40% toluene solution, 25.2 g) for 15 minutes, and the mixture was stirred at room temperature for 2 hours and concentrated under reduced pressure. To the residue was added diethylether, and insoluble materials were filtered off. The filtrate was washed with saturated brine and dried with magnesium sulfate. Under reduced pressure, the solvent was evaporated, and the residue was purified with silica gel column chromatography (ethyl acetate/hexane 1:5) and distilled under reduced pressure (1.5 mmHg, 190° C.) to give colorless oil of 4-bromo-3-chloro-(3-ethoxypropoxy)benzene (11.2 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06235771B1 |
|---|
| 출처 데이터셋 | uspto-grants-2001_05 |
|---|
| ORD ID | ord-27b5571bb6ef4756afb09de3f411e840 |
|---|
| 출처 메모 | uspto-grants-2001_05 |
|---|