Diethyl Ether → 1,3-Dichloro-3-fluoro-7-oxabicyclo[4.1.0]heptane
反応式
[OH-].[Na+].[Cl:3][C:4]1(Cl)[CH2:9][CH2:8][CH2:7][C:6]([Cl:11])([F:10])[CH:5]1O.CC[O:16]CC>O>[Cl:3][C:4]12[O:16][CH:9]1[CH2:8][CH2:7][C:6]([Cl:11])([F:10])[CH2:5]2参加物
5
実験手順
0.85 g (21.3 mmol) of sodium hydroxide pellets were added in three portions to 1.6 g (7.22 mmol) of pure alcohol 1f in suspension in 22 cm3 of distilled water at 15°-20° C. The reaction mixture was kept at room temperature for 1 h 15 min, 10 cm3 of ether were then added, stirring was continued for 5 min and then the aqueous phase was separated off and extracted with ether (5×25 cm3). The ether phases were combined, dried over magnesium sulfate and filtered, and the solvent was evaporated off. 1.28 g of a liquid, the epoxide 2e, were obtained; the crude yield was 96% (macrobore GC purity>98%).
後処理
- waitwas continued for 5 min
- customthe aqueous phase was separated off
- extractionextracted with ether (5×25 cm3)
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- customthe solvent was evaporated off
出典と根拠
- ORDレコード
- ord-5012092a33f94258a496fa5a096d1aad
- 出典データセット
- uspto-grants-1995_06
- 特許番号
- US05424460
反応ノート
読み込み中…