Potassium Hydroxide → 2,4-Bis(benzyloxy)-5-isopropenylbenzoic acid
Reaktionsgleichung
[OH-].[K+].[CH2:3]([O:10][C:11]1[CH:20]=[C:19]([O:21][CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[C:18]([C:29]([CH3:31])=[CH2:30])=[CH:17][C:12]=1[C:13]([O:15]C)=[O:14])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1>CO.O>[CH2:3]([O:10][C:11]1[CH:20]=[C:19]([O:21][CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[C:18]([C:29]([CH3:31])=[CH2:30])=[CH:17][C:12]=1[C:13]([OH:15])=[O:14])[C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1Komponenten
5
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 2
Reaktionsbedingungen
- Temperatur
- 40 °C
Versuchsvorschrift
Potassium hydroxide (0.527 Kg, 9.4 mol) was added to a stirred suspension of methyl 2,4-bis-benzyloxy-5-isopropenyl-benzoate (3.1 Kg, 8 mol, step 4) in methanol (18.6 L) and water (12.4 L) and the mixture was stirred and held at reflux for 3 hours. The methanol was removed under partial vacuum from the vessel, and to the remaining solution was added toluene (62 L). The solution was heated to 40° C. and to the mixture was added conc HCl (1.36 L). The biphasic mixture is heated to 50° C. and the phases separated. The organic phase was washed with water (31 L) at 50° C. and the organic phase was evaporated under reduced pressure to give 2,4-bis-benzyloxy-5-isopropenyl-benzoic acid 2.851 Kg (95% yield) as a colourless solid.
Aufarbeitung
- temperatureat reflux for 3 hours
- customThe methanol was removed under partial vacuum from the vessel
- additionto the remaining solution was added toluene (62 L)
- additionwas added conc HCl (1.36 L)
- temperatureThe biphasic mixture is heated to 50° C.
- customthe phases separated
- washThe organic phase was washed with water (31 L) at 50° C.
- customthe organic phase was evaporated under reduced pressure
Quellen und Nachweise
- ORD-Eintrag
- ord-da6685dae68c4bc89484b64383f38af6
- Quelldatensatz
- uspto-grants-2014_02
- Patentnummer
- US08653084B2
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