Methanol → methyl 2-(5-bromo-2-fluorophenyl)acetate
Reaktionsgleichung
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([F:12])=[C:6]([CH2:8][C:9]([OH:11])=[O:10])[CH:7]=1.S(=O)(=O)(O)O.[CH3:18]O>>[CH3:18][O:10][C:9](=[O:11])[CH2:8][C:6]1[CH:7]=[C:2]([Br:1])[CH:3]=[CH:4][C:5]=1[F:12]Komponenten
4
Reaktionsbedingungen
- Temperatur
- 64 °C
Versuchsvorschrift
To a solution of 5-bromo-2-fluorophenylacetic acid (5 g) in MeOH (200 mL) is added concentrated sulfuric acid (2 mL) and the solution is heated at 64° C. for 16 hours. The solution is evaporated in vacuo and the residue is taken up in EtOAc and washed with 10% sodium bicarbonate, brine and dried over sodium sulfate. The solution is filtered and evaporated in vacuo to afford (5-bromo-2-fluoro-phenyl)-acetic acid methyl ester (5.1 g). 1H NMR (300 MHz, CDCl3) □7.3-7.5 (m, 2H); 6.9 (m, 1H); 3.9 (s, 3H).
Aufarbeitung
- customThe solution is evaporated in vacuo
- washwashed with 10% sodium bicarbonate, brine
- dry with materialdried over sodium sulfate
- filtrationThe solution is filtered
- customevaporated in vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-9e574eeed79d45da9a30ccfbae9d5b6c
- Quelldatensatz
- uspto-grants-2012_06
- Patentnummer
- US08193183B2
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