N-bromobutanimide → HCID 66729043、化合物
反応式
[S:1]1[C:5]2[CH:6]=[C:7]([C:10]#[N:11])[CH:8]=[CH:9][C:4]=2[CH:3]=[CH:2]1.[Br:12]N1C(=O)CCC1=O>CN(C=O)C.O>[Br:12][C:3]1[C:4]2[CH:9]=[CH:8][C:7]([C:10]#[N:11])=[CH:6][C:5]=2[S:1][CH:2]=1参加物
5
実験手順
To a solution of 1-benzothiophene-6-carbonitrile (2.13 g, 13.4 mmol) in dry DMF (20 mL) at −10° C. was added freshly recrystallised N-bromosuccinimide (2.38 g, 13.4 mmol). The solution was allowed to warm to room temperature and stirred over the weekend. The mixture was diluted with water and extracted into diethyl ether, and the organic extract washed with water, then brine. The extracts were dried (MgSO4), filtered and evaporated in vacuo. The crude product was purified by flash chromatography on silica, eluting with ethyl acetate/hexane (1:9), to yield the title compound as a white solid.
後処理
- extractionextracted into diethyl ether
- extractionthe organic extract
- washwashed with water
- dry with materialThe extracts were dried (MgSO4)
- filtrationfiltered
- customevaporated in vacuo
- customThe crude product was purified by flash chromatography on silica
- washeluting with ethyl acetate/hexane (1:9)
出典と根拠
- ORDレコード
- ord-7ac78351942046b29770a41e6de5c8e3
- 出典データセット
- uspto-grants-2008_02
- 特許番号
- US07335660B2
反応ノート
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