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温度

0 °C

Racemic O-(phenylmethyl)serine (5 g, 25.6 mmol) and potassium bromide (10.7 g, 89.6 mmol) were dissolved in ice-cooled H2SO4 (2.5N) and treated with an solution of sodium nitrite (2.65 g) in water (30 ml) over 50 minutes (keeping the reaction temperature <4° C.). The reaction was then stirred at 0° C. for 45 minutes and then at rt for 1 h, extracted with ethyl acetate (3×100 ml). The combined organic extracts were washed with water, brine, dried (MgSO4), filtered and evaporated to give the product as a yellow oil (6 g, 90%).

1. customthe reaction temperature <4° C.
2. waitat rt for 1 h
3. extractionextracted with ethyl acetate (3×100 ml)
4. washThe combined organic extracts were washed with water, brine
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. customevaporated