反応式
C[Si](OS(C(F)(F)F)(=O)=O)(C)C.C[Si](C)(C)[O:15][CH2:16][CH2:17][O:18][Si](C)(C)C.O=[C:26]1[CH2:31][CH2:30][CH2:29][CH:28]([C:32]([O:34][CH3:35])=[O:33])[CH2:27]1>ClCCl>[O:15]1[C:26]2([CH2:31][CH2:30][CH2:29][CH:28]([C:32]([O:34][CH3:35])=[O:33])[CH2:27]2)[O:18][CH2:17][CH2:16]1参加物
5
反応条件
- 温度
- -78 °C
実験手順
To a solution of trimethylsilyltrifluoromethanesulfonate (0.034 mL) in dry dichloromethane (5 mL) was added 1,2-bis(trimethylsiloxy)ethane (4.55 mL) followed by methyl 3-oxocyclohexanecarboxylate (2.9 g). The reaction mixture was stirred for 3 hours at −78° C. The reaction mixture was quenched with dry pyridine (0.5 mL), poured into saturated aqueous NaHCO3, and extracted with ether. The ether layer was dried over Na2CO3/Na2SO4. The reaction mixture was concentrated and purified by flash chromatography on silica with 5 to 30% ethyl acetate in hexanes to provide the title compound.
後処理
- customThe reaction mixture was quenched with dry pyridine (0.5 mL)
- additionpoured into saturated aqueous NaHCO3
- extractionextracted with ether
- dry with materialThe ether layer was dried over Na2CO3/Na2SO4
- concentrationThe reaction mixture was concentrated
- custompurified by flash chromatography on silica with 5 to 30% ethyl acetate in hexanes
出典と根拠
- ORDレコード
- ord-9050507d09314ffca3406ac1c87e0adb
- 出典データセット
- uspto-grants-2013_11
- 特許番号
- US08580794B2
関連ノート
読み込み中…