Water → ethyl 6-bromo-2-methyl-4H-thieno[3,2-b]pyrrole-5-carboxylate
反応式
[CH3:1][C:2]1[S:9][C:8]2[CH:7]=[C:6]([C:10]([O:12][CH2:13][CH3:14])=[O:11])[NH:5][C:4]=2[CH:3]=1.[Br:15]N1C(=O)CCC1=O.O>O1CCCC1>[Br:15][C:7]1[C:8]2[S:9][C:2]([CH3:1])=[CH:3][C:4]=2[NH:5][C:6]=1[C:10]([O:12][CH2:13][CH3:14])=[O:11]参加物
5
実験手順
To a solution of ethyl 2-methyl-4H-thieno[3,2-b]pyrrole-5-carboxylate (1.0 g) in tetrahydrofuran (10 mL) was added N-Bromosuccinimide (0.94 g) under ice-cooling, and the mixture was stirred at the same temperature for 1 hour. To the reaction mixture was added water and the resulting mixture was extracted with ethyl acetate. The organic layer was concentrated under reduced pressure. The obtained residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate=97/3−76/24) to give the title compound (0.96 g).
後処理
- temperaturecooling
- extractionthe resulting mixture was extracted with ethyl acetate
- concentrationThe organic layer was concentrated under reduced pressure
- customThe obtained residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate=97/3−76/24)
出典と根拠
- ORDレコード
- ord-d7dfb078f25547c38e55d5827a6a83b6
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09115144B2
反応ノート
読み込み中…