Hydrochloric Acid → 3-Ethoxy-3-cyclobutene-1,2-dione
反応式
C([O:3][C:4]1(OCC)[C:7](OCC)([O:8][CH2:9][CH3:10])[CH2:6][C:5]1=[O:14])C.Cl>>[CH2:9]([O:8][C:7]1[C:4](=[O:3])[C:5](=[O:14])[CH:6]=1)[CH3:10]参加物
3
実験手順
##STR7## 45 g of 2,2,3,3-tetraethoxycyclobutanone are stirred vigorously at 50° C in 4 normal aqueous HCl until the starting material is no longer detectable. The reaction solution is then extracted for 20 hours continuously with diethyl ether and the organic extracts are dried over MgSO4 and concentrated. Precipitated crystals of 1-hydroxycyclobutene-3,4-dione are filtered off sharply and the liquid residue is distilled at 110° C/0.1 Torr to yield 6.65 g (=30% of theory) of the desired 1-ethoxycyclobutene-3,4-dione of the above structure.
後処理
- extractionThe reaction solution is then extracted for 20 hours continuously with diethyl ether
- dry with materialthe organic extracts are dried over MgSO4
- concentrationconcentrated
- customPrecipitated crystals of 1-hydroxycyclobutene-3,4-dione
- filtrationare filtered off sharply
- distillationthe liquid residue is distilled at 110° C/0.1 Torr
出典と根拠
- ORDレコード
- ord-196e75bb90e24370bbfbc5dcc3c35dfa
- 出典データセット
- uspto-grants-1978_05
- 特許番号
- US04092146
反応ノート
読み込み中…