Acetic Acid → 2-Pentenal, 2-methyl-4-phenyl-
反応式
[CH:1](=[O:4])[CH2:2][CH3:3].[C:5]1([CH:11]([CH3:14])[CH:12]=O)[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[OH-].[Na+].C(O)(=O)C>CO>[CH3:3][C:2](=[CH:12][CH:11]([CH3:14])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[CH:1]=[O:4]参加物
6
実験手順
192 g of propionaldehyde are added dropwise to a solution of 402 g of 2-phenylpropan-1-al and 12 g of sodium hydroxide in 1 l of methanol in the course of 6 hours. Stirring is continued for one hour, after which the mixture is neutralized with glacial acetic acid (pH=6), stirred overnight and evaporated down, the residue is taken up with CH2Cl2 /H2O, and the solution is extracted with CH2Cl2. The organic phase is washed with water, dried over Na2SO4, evaporated down again and distilled to give 178 g of 2,4-dimethyl-4-phenylbut-2-en-1-al of boiling point 108°-120° C./0.5 mbar.
後処理
- stirringstirred overnight
- customevaporated down
- extractionthe solution is extracted with CH2Cl2
- washThe organic phase is washed with water
- dry with materialdried over Na2SO4
- customevaporated down again
- distillationdistilled
出典と根拠
- ORDレコード
- ord-0f72f826f034420aaea23dd9c9ace2bb
- 出典データセット
- uspto-grants-1987_11
- 特許番号
- US04705553
反応ノート
読み込み中…