Ethanol → 5-Ethoxypyrimidine
反応式
[Na].Br[C:3]1[CH:4]=[N:5][CH:6]=[N:7][CH:8]=1.[CH2:9]([OH:11])[CH3:10]>>[CH2:9]([O:11][C:3]1[CH:4]=[N:5][CH:6]=[N:7][CH:8]=1)[CH3:10]参加物
4
実験手順
Sodium (2.89 g. 125.8 mmol) was dissolved in ethanol (110 mL) and 5-bromopyrimidine (10.0 g, 62.9 mmol) added. The reaction was heated at 120° in an autoclave for 17 h and then allowed to stand at 23° for 60 h. The ethanol was removed under reduced pressure and water (5 mL) added to the concentrate. The aqueous phase was extracted with CH2Cl2 (4×100 mL). The combined organic extracts were washed with saturated NaCl solution, dried with anhydrous K2CO3, filtered, and concentrated under reduced pressure. Silica gel chromatography (Hexane/EtOAc; 70:30) of the concentrate yielded 5-ethoxypyrimidine (2.00 g, 25.6%).
後処理
- temperatureThe reaction was heated at 120° in an autoclave for 17 h
- customThe ethanol was removed under reduced pressure and water (5 mL)
- additionadded to the concentrate
- extractionThe aqueous phase was extracted with CH2Cl2 (4×100 mL)
- washThe combined organic extracts were washed with saturated NaCl solution
- dry with materialdried with anhydrous K2CO3
- filtrationfiltered
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-77972697092b4fd59903f046ff5a45d4
- 出典データセット
- uspto-grants-1995_07
- 特許番号
- US05434154
反応ノート
読み込み中…