Trifluoroacetic acid → HCID 86692460、化合物
反応式
FC(F)(F)C(O)=O.[Br:8][C:9]1[CH:10]=[CH:11][C:12]([C:15]2([C:25]#[N:26])[CH2:24][CH2:23][C:18]3(OCC[O:19]3)[CH2:17][CH2:16]2)=[N:13][CH:14]=1>>[Br:8][C:9]1[CH:10]=[CH:11][C:12]([C:15]2([C:25]#[N:26])[CH2:16][CH2:17][C:18](=[O:19])[CH2:23][CH2:24]2)=[N:13][CH:14]=1参加物
3
実験手順
Trifluoroacetic acid (4.1 ml) was added to 8-(5-bromopyridin-2-yl)-1,4-dioxaspiro[4,5]decane-8-carbonitrile (3.4 g) described in Reference Example 82 at room temperature, and stirred at the same temperature for 22 hours. After completion of the reaction, the solvent and trifluoroacetic acid were evaporated and the resulting residue was purified with silica gel column chromatography (n-hexane/ethyl acetate) to give 1-(5-bromopyridin-2-yl)-4-oxocyclohexanecarbonitrile (2.78 g) as a white solid.
後処理
- customdescribed in Reference Example 82 at room temperature
- customAfter completion of the reaction
- customthe solvent and trifluoroacetic acid were evaporated
- customthe resulting residue was purified with silica gel column chromatography (n-hexane/ethyl acetate)