Reaktionsgleichung
[Br:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][C:11]([OH:13])=[O:12].[CH2:14](O)[CH3:15]>>[Br:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12]Komponenten
Versuchsvorschrift
To this end, the 180.5 g of 10-bromodecanoic acid from Step II was added to the 11 reactor (described above) along with 645 g of absolute ethanol. The mixture was heated and stirred for about 3.5 h. GC analysis confirmed that reaction was completed when 10-bromodecanoic acid could not be detected. Next, excess ethanol and residual water were removed through evaporation leaving 197.8 g of 94.9% pure ethyl 10-bromodecanoate residue. 150 g MTBE was added to the ethyl 10-bromodecanoate residue which then was washed repeatedly with 10% sodium carbonate solution followed by water. The mixture was phase separated to obtain 340.7 g of a mixture of ethyl 10-bromodecanoate and MTBE. According to GC analysis the yield from Steps II and III was 89.7%.
Aufarbeitung
- temperatureThe mixture was heated
- customGC analysis confirmed that reaction
- customNext, excess ethanol and residual water were removed through evaporation
Quellen und Nachweise
- ORD-Eintrag
- ord-743cfd1475e8481ba3391b1b90f473f5
- Quelldatensatz
- uspto-grants-2001_01
- Patentnummer
- US06175024B1
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