反应详情

温度

-5 °C

Mix D-phenylalanine (186.4g, 1.128mol) and 49% hydrobromic acid (372.8g), cool to -5° C. and add, by dropwise addition, a solution of sodium nitrite (77.9g) in water (565mL) over a period of about 1 hour (vigorous gas evolution). Stir at -5° C. to 0° C. for 4 hours, extract into ethyl ether (3×1L), dry (MgSO4) and evaporate the solvent in vacuo. Purify by chromatography (5% acetic aci/95% methylene chloride) and distillation to give 3-phenyl-2(R)-bromopropionic acid (112g, 43%); bp 128°-135° C. @0.25 torr.

1. additionadd, by dropwise addition
2. extractionextract into ethyl ether (3×1L)
3. dry with materialdry (MgSO4)
4. customevaporate the solvent in vacuo
5. distillationPurify by chromatography (5% acetic aci/95% methylene chloride) and distillation