Hydrochloric Acid → 3-(2',4',5'-Triethoxybenzoyl)-trans-acrylic acid
Reaktionsgleichung
[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([O:10][CH2:11][CH3:12])=[CH:6][C:5]=1[O:13][CH2:14][CH3:15])[CH3:2].[C:16]1(=[O:22])[O:21][C:19](=[O:20])[CH:18]=[CH:17]1.[Cl-].[Al+3].[Cl-].[Cl-].Cl>C(Cl)(Cl)(Cl)Cl>[CH2:11]([O:10][C:7]1[CH:6]=[C:5]([O:13][CH2:14][CH3:15])[C:4]([O:3][CH2:1][CH3:2])=[CH:9][C:8]=1[C:16](/[CH:17]=[CH:18]/[C:19]([OH:21])=[O:20])=[O:22])[CH3:12]Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 50 °C
Versuchsvorschrift
To a mixture of 2.1 parts by weight of 1,2,4-triethoxybenzene, 1.2 parts by weight of maleic anhydride and 30 parts by volume of carbon tetrachloride is added 5.2 parts by weight of anhydrous aluminum chloride. The mixture is stirred for 1 hour and heated at 50° C. for another 1 hour. After cooling, concentrated hydrochloric acid and ice are added to the mixture. The mixture is extracted with methylenechloride and the methylenechloride layer is washed with water and dried over anhydrous sodium sulfate. Upon removing the solvent by distillation, 3-(2',4',5'-triethoxybenzoyl)-trans-acrylic acid is obtained as crystals. Recrystallization from a mixture of ethanol and benzene gives yellow needles melting at 192°-194° C.
Aufarbeitung
- temperatureAfter cooling
- extractionThe mixture is extracted with methylenechloride
- washthe methylenechloride layer is washed with water
- dry with materialdried over anhydrous sodium sulfate
- customUpon removing the solvent
- distillationby distillation
Quellen und Nachweise
- ORD-Eintrag
- ord-4cb5bf52ccb242a3b83954713b1b8801
- Quelldatensatz
- uspto-grants-1977_06
- Patentnummer
- US04029699
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