反応式
[N:1]1[C:10]2[C:5](=[CH:6][C:7]([C:11]([NH2:13])=O)=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.C(N(CC)CC)C.FC(F)(F)C(OC(=O)C(F)(F)F)=O>C(Cl)Cl>[N:1]1[C:10]2[C:5](=[CH:6][C:7]([C:11]#[N:13])=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1参加物
5
反応条件
- 温度
- 0 °C
実験手順
Dissolve 6-quinolinecarboxamide (1.5 g, 8.95 mmol) in DCM (50 mL), add triethylamine (2.7 g, 26.8 mmol) and cool the reaction mixture to 0° C. Add trifluoroacetic acid anhydride (2.4 g, 11.16 mmol) to the reaction mixture and stir for 10 min at 0° C. Quench the reaction mixture with water (20 mL) and separate the organic layer. Extract aqueous layer with DCM (2×15 mL). Combine the organic extracts and dry over anhydrous Na2SO4. Evaporate the solvent to obtain the desired intermediate as a white solid (1.0 g, 73%). GC-MS m/z: 154 (M+).
後処理
- customQuench the reaction mixture with water (20 mL)
- customseparate the organic layer
- dry with materialCombine the organic extracts and dry over anhydrous Na2SO4
- customEvaporate the solvent
出典と根拠
- ORDレコード
- ord-33fd24d558904523b3b4f91e87c9b34e
- 出典データセット
- uspto-grants-2011_09
- 特許番号
- US08022062B2
関連ノート
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