Cycloheptanone → 1-Oxaspiro(2.6)nonane
反応式
[I-].C[S+](C)C.[C:6]1(=[O:13])[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1.[CH3:14]C(C)([O-])C.[K+]>CS(C)=O>[O:13]1[C:6]2([CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]2)[CH2:14]1参加物
5
実験手順
To a mixture of trimethylsulfonium iodide (35.7 g) in 300 mL dry DMSO was added 11.2 g of cycloheptanone with stirring. A solution of potassium tert-butoxide (16.83 g) in 200 mL dry DMSO was slowly added. The resulting solution was stirred at room temperature for 16 hours. The reaction mixture was quenched by addition of water (600 mL), and extracted with diethyl ether (3×200 mL). The combined organic layers were washed with water (200 mL), dried over Na2SO4, filtered, and concentrated under reduced pressure to give the product.
後処理
- stirringThe resulting solution was stirred at room temperature for 16 hours
- customThe reaction mixture was quenched by addition of water (600 mL)
- extractionextracted with diethyl ether (3×200 mL)
- washThe combined organic layers were washed with water (200 mL)
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- customto give the product
出典と根拠
- ORDレコード
- ord-013fb8225341426c88f999078c014c2b
- 出典データセット
- uspto-grants-2015_01
- 特許番号
- US08940737B2
反応ノート
読み込み中…