反応式
[CH3:1][O:2][CH:3]([O:12][CH3:13])[C:4]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[CH:6][CH:5]=1.C1(C)C=CC(S(O)(=O)=O)=CC=1.C(N(CC)CC)C.[C:32]([O:35][CH2:36][CH3:37])(=O)C.C[C:39](N(C)C)=[O:40]>>[CH3:11][O:10][C:7]1[CH:8]=[CH:9][C:4]([C@@H:3]2[O:12][CH2:13][C@@H:32]3[C@H:1]([C@H:39]([OH:40])[CH2:37][CH2:36][O:35]3)[O:2]2)=[CH:5][CH:6]=1参加物
反応条件
- 温度
- 62.5 °C
実験手順
5.0 g (33.8 mmol) of 2 and 8.30 g (45.8 mmol) of p-methoxybenzaldehyde dimethyl acetal were dissolved in 50 ml of anhydrous DMA, and a catalytic amount of 4-toluenesulfonic acid was added until the mixture was acidic. The reaction solution was agitated for about 5 hours in a rotary evaporator at 60-65° C. and a reduced pressure of 30 mbar. The reaction solution was neutralized using triethylamine. 300 ml of ethyl acetate were added, and the mixture was extracted three times with water. The organic phase was dried over Na2SO4, the drying agent was filtered off, and the residue was evaporated under reduced pressure. The crude product was dissolved in a little ethyl acetate, precipitated using n-hexane, filtered off with suction and dried under reduced pressure.
後処理
- extractionthe mixture was extracted three times with water
- dry with materialThe organic phase was dried over Na2SO4
- filtrationthe drying agent was filtered off
- customthe residue was evaporated under reduced pressure
- dissolutionThe crude product was dissolved in a little ethyl acetate
- customprecipitated
- filtrationfiltered off with suction
- customdried under reduced pressure
出典と根拠
- ORDレコード
- ord-63a9c62168864f38bdd617b0cdcec539
- 出典データセット
- uspto-grants-2003_05
- 特許番号
- US06569355B1
関連ノート
読み込み中…