Hydrochloric Acid → 6-fluoro-4-cyano-2H-benzopyran
반응식
[F:1][C:2]1[CH:3]=[CH:4][C:5]2[O:10][CH2:9][CH2:8][C:7]([C:16]#[N:17])(O[Si](C)(C)C)[C:6]=2[CH:18]=1.P(Cl)(Cl)(Cl)=O.Cl>N1C=CC=CC=1.O>[F:1][C:2]1[CH:3]=[CH:4][C:5]2[O:10][CH2:9][CH:8]=[C:7]([C:16]#[N:17])[C:6]=2[CH:18]=1참가 물질
6
실험 절차
To a solution of 32 g (0.12 mole) of the crude 6-fluoro-2,3-dihydro-4-cyano-4-[(trimethylsilyl)oxy]-4H-benzopyran in 170 ml of dry pyridine was added 60 ml (0.6 mole) of phosphorous oxychloride. The reaction was heated to reflux for 5 hours then cooled to room temperature. The resulting solution was added dropwise to a solution of 300 cc of concentrated HCl in 1 L of water. This aqueous layer was extracted with EtOAc and the EtOAc layer was dried over Na2SO4, filtered and evaporated to give 16.1 g of product m.p. 114°-115° C.
후처리
- temperatureThe reaction was heated
- temperatureto reflux for 5 hours
- extractionThis aqueous layer was extracted with EtOAc
- dry with materialthe EtOAc layer was dried over Na2SO4
- filtrationfiltered
- customevaporated
출처 및 근거
- ORD 기록
- ord-d9f23d4a2b63445484305e40cb15637e
- 출처 데이터셋
- uspto-grants-1994_03
- 특허 번호
- US05294635
반응 노트
불러오는 중…