反応式
Br[C:2]1[CH:3]=[N:4][CH:5]=[CH:6][CH:7]=1.[CH3:8][CH:9]([OH:13])[CH2:10][CH:11]=[CH2:12].C(N(CC)CC)C.C(#N)C>O.C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C1(C)C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C>[N:4]1[CH:5]=[CH:6][CH:7]=[C:2](/[CH:12]=[CH:11]/[CH2:10][CH:9]([OH:13])[CH3:8])[CH:3]=1参加物
8
反応条件
- 温度
- 140 °C
実験手順
A mixture of 3-bromopyridine (7.50 g, 47.46 mmol), 4-penten-2-ol (4.90 g, 56.96 mmol), palladium(II) acetate (106 mg, 0.47 mmol), tri-o-tolylphosphine (575 mg, 1.89 mmol), triethylamine (28.4 mL, 204.11 mmol) and acetonitrile (25 mL) were heated in a sealed glass tube at 140° C. for 14 h. The reaction mixture was cooled to ambient temperature, diluted with water, and extracted with chloroform (3×200 mL). The combined chloroform extracts were dried over sodium sulfate, filtered, and concentrated by rotary evaporation to give a pale-yellow oil (7.50 g, 81.0%).
後処理
- temperatureThe reaction mixture was cooled to ambient temperature
- extractionextracted with chloroform (3×200 mL)
- dry with materialThe combined chloroform extracts were dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated by rotary evaporation
出典と根拠
- ORDレコード
- ord-feffb67306e446c1b0a403b902105424
- 出典データセット
- uspto-grants-2005_12
- 特許番号
- US06979695B2
関連ノート
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