Potassium Bromide → (S)-2-bromo-4-methylpentanoic acid

Temperature

-10 °C

Potassium bromide (9.5 g., 80 mmol.) was added to a stirred solution of D-leucine (3.0 g., 23 mmol.) in 2.5N sulfuric acid (47 ml.) at room temperature. The reaction mixture was cooled to -10° C. and solid sodium nitrite (2.4 g., 34 mmol.) was added portionwise, maintaining the temperature between -10° and -5° C. After addition was complete, the reaction was stirred for 1 hour and then warmed to room temperature and stirred for another hour. The reaction mixture was then extracted twice with ether, the ether extracts were washed once with water, dried (magnesium sulfate), filtered and evaporated to give 2.7 g. of crude title product.

1. temperaturemaintaining the temperature between -10° and -5° C
2. additionAfter addition
3. temperaturewarmed to room temperature
4. stirringstirred for another hour
5. extractionThe reaction mixture was then extracted twice with ether
6. washthe ether extracts were washed once with water
7. dry with materialdried (magnesium sulfate)
8. filtrationfiltered
9. customevaporated
10. customto give 2.7 g

ORD record

ord-f61706e6f3f34088a315daa06993d596

Source dataset

uspto-grants-1997_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05646276