反応式
[CH3:1][N:2]([CH3:8])[C@H:3]1[CH2:7][CH2:6][NH:5][CH2:4]1.C(N(CC)CC)C.[Br:16][C:17]1[C:18](F)=[C:19]2[O:23][C:22]([CH:24]3[CH2:26][CH2:25]3)=[N:21][C:20]2=[C:27]([C:30]#[N:31])[C:28]=1[CH3:29]>CS(C)=O>[Br:16][C:17]1[C:18]([N:5]2[CH2:6][CH2:7][C@H:3]([N:2]([CH3:8])[CH3:1])[CH2:4]2)=[C:19]2[O:23][C:22]([CH:24]3[CH2:25][CH2:26]3)=[N:21][C:20]2=[C:27]([C:30]#[N:31])[C:28]=1[CH3:29]参加物
反応物 3
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 90 °C
実験手順
(3S)-3-(Dimethylamino)pyrrolidine (157 μl, 1.24 mmol) and triethylamine (348 μl, 2.50 mmol), were added to a dimethyl sulfoxide (5 ml) solution of 6-bromo-2-cyclopropyl-7-fluoro-5-methyl-1,3-benzoxazole-4-carbonitrile (I-77) (304 mg, 1.03 mmol). The system was purged with nitrogen and then sealed up and heated at 90° C. for 2 hours. After cooling, the solvent was evaporated away under reduced pressure, then the resulting residue was dissolved in chloroform, washed with water and saturated brine. The organic layer was dried over anhydrous sodium sulfate, then the solvent was evaporated away under reduced pressure, the resulting residue was washed with a mixed solvent of isopropyl ether and ethanol. The crystal was collected by filtration to obtain the entitled compound (106 mg, 26%) as a colorless solid.
後処理
- customThe system was purged with nitrogen
- customsealed up
- temperatureAfter cooling
- customthe solvent was evaporated away under reduced pressure
- dissolutionthe resulting residue was dissolved in chloroform
- washwashed with water and saturated brine
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- customthe solvent was evaporated away under reduced pressure
- washthe resulting residue was washed with a mixed solvent of isopropyl ether and ethanol
- filtrationThe crystal was collected by filtration
出典と根拠
- ORDレコード
- ord-5089e38f65e34a179fddb8f70be12570
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07737166B2
関連ノート
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