Ethanol → 2-Fluoro-3,4-dihydroxy-5-nitrobenzonitrile
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[F:1][C:2]1[C:9]([OH:10])=[C:8]([O:11]C)[C:7]([N+:13]([O-:15])=[O:14])=[CH:6][C:3]=1[C:4]#[N:5].B(Br)(Br)Br.C(O)C>C(Cl)Cl>[F:1][C:2]1[C:9]([OH:10])=[C:8]([OH:11])[C:7]([N+:13]([O-:15])=[O:14])=[CH:6][C:3]=1[C:4]#[N:5]참가 물질
5
실험 절차
550 mg of 2-fluoro-3-hydroxy-5-nitro-p-anisonitrile are dissolved in 30 ml of methylene chloride, whereupon the solution is treated with 0.44 ml of boron tribromide. After stirring at 23° for 6 hours an additional 0.1 ml of boron tribromide are added thereto, whereupon the mixture is stirred at 23° for an additional 1.5 hours. Thereupon, 3 ml of ethanol are added thereto at -15°. The reaction mixture is evaporated and the residue is dried in a high vacuum at 23°. By recrystallization from ether/hexane there is obtained 2-fluoro-3,4-dihydroxy-5-nitrobenzonitrile of m.p. 154°.
후처리
- additionare added
- customat -15°
- customThe reaction mixture is evaporated
- customthe residue is dried in a high vacuum at 23°
- customBy recrystallization from ether/hexane there
출처 및 근거
- ORD 기록
- ord-abef29f5caa94a9cb778712b3fff66cd
- 출처 데이터셋
- uspto-grants-1997_05
- 특허 번호
- US05633371
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