Dimethyl Sulfoxide → 1255713-68-8
反応式
[Br:1][C:2]1[C:3]([F:12])=[CH:4][C:5]2[O:9][C:8](=[O:10])[NH:7][C:6]=2[CH:11]=1.[CH3:13]S(C)=O.CI.C(=O)([O-])[O-].[K+].[K+]>O>[Br:1][C:2]1[C:3]([F:12])=[CH:4][C:5]2[O:9][C:8](=[O:10])[N:7]([CH3:13])[C:6]=2[CH:11]=1参加物
6
実験手順
A flask was charged with 5-bromo-6-fluorobenzo[d]oxazol-2(3H)-one (3.6 g, 14.74 mmol) and DMSO (150 mL), and MeI (4.18 g, 29.5 mmol) and potassium carbonate (5.09 g, 36.9 mmol) were added. The mixture was stirred at room temperature overnight. The mixture was poured to water (1.2 L) and the precipitate was filtered, washed with water and dried under high vacuum at 60° C. for 1 h to give 5-bromo-6-fluoro-3-methylbenzo[d]oxazol-2(3H)-one. 1H NMR (400 MHz, DMSO-d6) δ ppm 3.32 (s, 3H) 7.62 (d, J=8.34 Hz, 1H) 7.70 (d, J=6.06 Hz, 1H).
後処理
- additionwere added
- filtrationthe precipitate was filtered
- washwashed with water
- customdried under high vacuum at 60° C. for 1 h
出典と根拠
- ORDレコード
- ord-b6ddd81ca7cd4c4386eac7164d8dd5f0
- 出典データセット
- uspto-grants-2013_06
- 特許番号
- US08455522B2
反応ノート
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