Acetic Anhydride → 3-Chloro-4-acetoxybenzoic acid
Reaktionsgleichung
[OH:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[Cl:11].[C:12](OC(=O)C)(=[O:14])[CH3:13]>>[C:12]([O:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[Cl:11])(=[O:14])[CH3:13]Komponenten
3
Versuchsvorschrift
A mixture of 10 g. 4-hydroxy-3-chlorobenzoic acid and 50 ml. of acetic anhydride is refluxed for two hours. Excess acetic anhydride is distilled under vacuum and the residue diluted and stirred with a mixture of methanol (100 ml.) and water (20 ml.) at about 50° for 30 minutes. The mixture is then reduced to low volume under vacuum, water added and the precipitated crystals filtered. Recrystallization from toluene gives 6.5 g. (52% yield) m.p. 162°-163° C.
Aufarbeitung
- additionA mixture of 10 g
- distillationExcess acetic anhydride is distilled under vacuum
- additionthe residue diluted
- additionadded
- filtrationthe precipitated crystals filtered
- customRecrystallization from toluene
- customgives 6.5 g
Quellen und Nachweise
- ORD-Eintrag
- ord-719aea01a4cf40cf9d75d0c5817b5ac9
- Quelldatensatz
- uspto-grants-1979_04
- Patentnummer
- US04151297
Notizen zur Reaktion
Wird geladen…