반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[OH:9].[Br:10]N1C(=O)CCC1=O>CN(C=O)C>[Br:10][C:6]1[CH:7]=[C:2]([F:1])[C:3]([OH:9])=[C:4]([F:8])[CH:5]=1참가 물질
4
실험 절차
To a solution of 2,6-Difluorophenol (10.0 g, 76.86 mmoles) in DMF (60 mll), N-bromosuccinimide (13.68 g, 76.86 mmoles) was added at 0° C. and stirred at RT for 20 h. The reaction mixture was concentrated, diluted with water and extracted with ethyl acetate. The organic layer was dried over sodium sulphate and concentrated under reduced pressure to afford the title compound as light yellow liquid (15.1 g, 93% yield). 1H-NMR (δ ppm, DMSO-D6, 400 MHz): δ 10.49(s,1H), 7.35 (d, J=6.2 Hz, 2H).
후처리
- concentrationThe reaction mixture was concentrated
- additiondiluted with water
- extractionextracted with ethyl acetate
- dry with materialThe organic layer was dried over sodium sulphate
- concentrationconcentrated under reduced pressure
출처 및 근거
- ORD 기록
- ord-7b7b34e3215946ff84a451c1b98d85db
- 출처 데이터셋
- uspto-grants-2014_02
- 특허 번호
- US08642607B2
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