反応式
[CH3:1][O:2][C:3]1[C:8]2[N:9]=[C:10]([C:12]3([CH3:17])[O:16][CH2:15][CH2:14][O:13]3)[O:11][C:7]=2[CH:6]=[CH:5][CH:4]=1.[Br:18]N1C(=O)CCC1=O>C(#N)C>[Br:18][C:6]1[C:7]2[O:11][C:10]([C:12]3([CH3:17])[O:16][CH2:15][CH2:14][O:13]3)=[N:9][C:8]=2[C:3]([O:2][CH3:1])=[CH:4][CH:5]=1参加物
4
実験手順
4-Methoxy-2-(2-methyl-[1,3]-dioxolan-2-yl)benzoxazole (129 m), N-bromosuccinimide (107 mg) and acetonitrile (5 ml) were combined and stirred at room temperature under nitrogen for 4 h. The mixture was partitioned between water (20 ml) and ethyl acetate (20 ml). The aqueous phase was extracted with ethyl acetate (20 ml). The combined organic phases were washed with water (2×50 ml), dried over magnesium sulphate, evaporated in vacuo and purified by flash chromatography eluting with 30% ethyl acetate in hexane to yield the title compound as a white solid (95 mg).
後処理
- customThe mixture was partitioned between water (20 ml) and ethyl acetate (20 ml)
- extractionThe aqueous phase was extracted with ethyl acetate (20 ml)
- washThe combined organic phases were washed with water (2×50 ml)
- dry with materialdried over magnesium sulphate
- customevaporated in vacuo
- custompurified by flash chromatography
- washeluting with 30% ethyl acetate in hexane
出典と根拠
- ORDレコード
- ord-8f21f728eb914cf399d730d3f86ffecc
- 出典データセット
- uspto-grants-2002_03
- 特許番号
- US06353010B1
関連ノート
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