反応式
Br[C:2]1[CH:3]=[C:4]([O:8][CH:9]([CH3:11])[CH3:10])[CH:5]=[N:6][CH:7]=1.[CH3:12][C@@H:13]([OH:17])[CH2:14][CH:15]=[CH2:16].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>[CH:9]([O:8][C:4]1[CH:3]=[C:2](/[CH:16]=[CH:15]/[CH2:14][C@H:13]([OH:17])[CH3:12])[CH:7]=[N:6][CH:5]=1)([CH3:11])[CH3:10]参加物
8
反応条件
- 温度
- 140 °C
実験手順
A mixture of 5-bromo-3-isopropoxypyridine (10.26 g, 47.50 mmol), (2R)-4-penten-2-ol (4.91 g, 57.00 mmol), palladium(II) acetate (106 mg, 0.47 mmol), tri-o-tolylphosphine (578 mg, 1.90 mmol), triethylamine (28.46 mL, 204.25 mmol), and acetonitrile (30 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 (8.92 g, 85.0%).
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-e15117959d294ed599fbdee22e3c4bd1
- 出典データセット
- uspto-grants-2001_04
- 特許番号
- US06218383B1
関連ノート
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