Methanol → Methyl 4-bromo-2-methylbutanoate

4-Bromo-2-methyl-butyric acid (2.16 g, 1 eq, prepared according to the procedure described in J. Am. Chem. Soc. 1990, 112, 2755) was dissolved in MeOH (10 mL) and a few drops of conc. H2SO4 were added. The reaction was stirred at reflux for 16 hours. After reaction completion, as monitored by LC-MS, MeOH was removed under reduced pressure, the oily residue was diluted with water, the pH adjusted to 9 with 10% NaOH, and the product was extracted with Et2O (2×20 mL) and dried over Na2SO4. The title compound was obtained as a colourless oil (1.29 g, 55% yield) after solvent removal.

1. temperatureat reflux for 16 hours
2. customAfter reaction completion
3. customwas removed under reduced pressure
4. additionthe oily residue was diluted with water
5. extractionthe product was extracted with Et2O (2×20 mL)
6. dry with materialdried over Na2SO4

ORD-Eintrag

ord-d5c6090c33fe4d359128fb48e8792ec7

Quelldatensatz

uspto-grants-2012_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08163729B2