反応式
[CH3:1][N:2]([CH3:20])[C:3]([C:5]1[O:6][C:7]2[C:13]([N:14]3[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]3)=[CH:12][CH:11]=[CH:10][C:8]=2[CH:9]=1)=[O:4].C(O)(=O)C.[F:25][C:26]([F:36])([F:35])[C:27]1[CH:32]=[CH:31][CH:30]=[C:29]([CH:33]=[CH2:34])[N:28]=1>C(O)C>[CH3:1][N:2]([CH3:20])[C:3]([C:5]1[O:6][C:7]2[C:13]([N:14]3[CH2:19][CH2:18][N:17]([CH2:34][CH2:33][C:29]4[CH:30]=[CH:31][CH:32]=[C:27]([C:26]([F:36])([F:25])[F:35])[N:28]=4)[CH2:16][CH2:15]3)=[CH:12][CH:11]=[CH:10][C:8]=2[CH:9]=1)=[O:4]参加物
反応条件
- 温度
- 73 °C
実験手順
N,N-dimethyl-7-(piperazin-1-yl)benzofuran-2-carboxamide (0.09 g, 0.33 mmol) (Example 39d) was dissolved in ethanol (0.95 mL), and acetic acid (0.015 mL, 0.26 mmol) was added, followed by 2-(trifluoromethyl)-6-vinylpyridine (0.10 g, 0.58 mmol) (volatile) dissolved in ethanol (1.40 mL). The mixture was heated at 73° C. for 14 h in the microwave and then heated for another 48 h at 86° C. in an oilbath, and finally it was heated in the microwave for 15 min at 100° C. More 2-(trifluoromethyl)-6-vinylpyridine (0.10 g, 0.58 mmol) and ethanol (0.95 mL) were added and the mixture was heated in a oil bath for 7 days at 86° C. The product was purified by flash chromatography (SiO2; DCM/MeOH; gradient 0-7%) and then by preparative HPLC to give the title compound. Yield: 0.075 g (51%).
後処理
- temperatureheated for another 48 h at 86° C. in an oilbath, and finally it
- temperaturewas heated in the microwave for 15 min at 100° C
- temperaturethe mixture was heated in a oil bath for 7 days at 86° C
- customThe product was purified by flash chromatography (SiO2; DCM/MeOH; gradient 0-7%)
出典と根拠
- ORDレコード
- ord-acdce69150ff404f823ef7801f7302b1
- 出典データセット
- uspto-grants-2014_10
- 特許番号
- US08859534B2
関連ノート
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