1-Bromo-3,5-difluorobenzene → 1-Bromo-3-fluoro-5-(methylsulfanyl)benzene
반응식
[Br:1][C:2]1[CH:7]=[C:6](F)[CH:5]=[C:4]([F:9])[CH:3]=1.[CH3:10][S-:11].[Na+]>CN(C)C=O>[Br:1][C:2]1[CH:7]=[C:6]([S:11][CH3:10])[CH:5]=[C:4]([F:9])[CH:3]=1참가 물질
4
반응 조건
- 온도
- 150 °C
실험 절차
To a solution of 1-bromo-3,5-difluorobenzene (5.0 g, 25.9 mmol) in dimethylformamide (40 ml) was added sodiumthiomethylate (1.81 g, 25.9 mmol), and the mixture was heated to 150° C. for 10 min. The reaction mixture was brought to ambient temperature, quenched with saturated aqueous ammonium chloride (100 ml) and extracted with ethylacetate (3×100 ml). The combined organic phases was dried and concentrated in vacuo to receive the pure title compound (3.84 g). MS m/z (rel. intensity, 70 eV) 222 (M+, 100), 220 (M+, 100), 189 (49), 187 (50), 126 (75).
후처리
- customwas brought to ambient temperature
- customquenched with saturated aqueous ammonium chloride (100 ml)
- extractionextracted with ethylacetate (3×100 ml)
- customThe combined organic phases was dried
- concentrationconcentrated in vacuo
출처 및 근거
- ORD 기록
- ord-ef19c52ec3fb43ea8415c457ee1025ab
- 출처 데이터셋
- uspto-grants-2013_08
- 특허 번호
- US08501777B2
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