Diethyl Ether → 3-Butylfuran
反応式
C([Li])(C)(C)C.[CH3:6][CH2:7][CH2:8][CH2:9]C.[CH3:11][CH2:12][O:13][CH2:14][CH3:15]>>[CH2:6]([C:11]1[CH:15]=[CH:14][O:13][CH:12]=1)[CH2:7][CH2:8][CH3:9]参加物
4
反応条件
- 温度
- -78 °C
実験手順
The iodo-product obtained from Step B above (2.2 g, 8.8 mmol) was dissolved in 60 mL of ether, and stirred in a −78° C. bath. A 1.7 M solution of t-butyllithium in pentane (10.4 mL, 17.7 mmol) was added dropwise. After 20 min, cooling bath was removed. Reaction was continued for 2.5 h, and quenched with H2O (20 mL). The aqueous mixture was stirred overnight and separated. The aqueous layer was extracted with ether (30 mL). The combined organic layers were washed with brine, dried by Na2SO4, and filtered through a Celite pad. Removal of solvent gave 1.10 g (100%) of 3-butylfuran as a reddish-yellow oil.
後処理
- temperaturecooling bath
- customwas removed
- customReaction
- waitwas continued for 2.5 h
- customquenched with H2O (20 mL)
- stirringThe aqueous mixture was stirred overnight
- customseparated
- extractionThe aqueous layer was extracted with ether (30 mL)
- washThe combined organic layers were washed with brine
- dry with materialdried by Na2SO4
- filtrationfiltered through a Celite pad
- customRemoval of solvent
出典と根拠
- ORDレコード
- ord-d686f14f606c4634a4f8638e75e304b3
- 出典データセット
- uspto-grants-2006_11
- 特許番号
- US07132445B2
反応ノート
読み込み中…