Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sulfuric Acid → 1-[Bis(4-fluorophenyl)methoxy]-4-chlorobutane
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sulfuric Acid | HCID 1118 | — |
| 반응물 | 4-Chloro-1-butanol | HCID 13569 | — |
| 반응물 | 4,4'-Difluorobenzhydryl alcohol | HCID 123049 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 1-[Bis(4-fluorophenyl)methoxy]-4-chlorobutane | HCID 10757372 | 75% |
반응 단계
A mixture of 4-chloro-1-butanol (6.51 g, 60 mmol), 1 mL of concentrated sulfuric acid and 4,4′-difluorobenzhydrol (2.2 g, 10 mmol) in 50 mL of toluene was heated at reflux for 12 h. The reaction mixture was cooled, washed successively with saturated sodium bicarbonate solution (50 mL) and water (50 mL). The organic layer was dried over MgSO4, filtered and the solvent was removed by rotary evaporation. The resultant brown oil was purified on a silica gel column. Elution with 2% ethyl acetate/hexane afforded 2.33 g (7.5 mmol, 75%) of the product as a colorless oil. 1H NMR (CDCl3): δ 1.71-1.80 (2H, m), 1.84-1.93 (2H, m), 3.43 (2H, t, J=6.0), 3.52 (2H, t, J=6.4), 5.30 (1H, s) 6.95-7.02 (4H, m), 7.24-7.29 (4H, m)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08772319B2 |
| 출처 데이터셋 | uspto-grants-2014_07 |
| ORD ID | ord-16b3a2696f5f4829a67fa7fcb42a0509 |
| 출처 메모 | uspto-grants-2014_07 |