HRID982569

反应详情

EQUATION

反应方程式

HRID 982569 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.85 g of isobutylacrylic acid and 10.9 g of O-benzylhydroxylamine were heated under reflux in 30 ml of methanol for 8 days. The solvent was removed by evaporation and the residue was dissolved in ethyl acetate and water. The organic layer was washed with 2N hydrochloric acid and water and then extracted six times with 30 ml of 5% sodium hydrogen carbonate solution each time. The aqueous solutions were combined, acidified with 2N hydrochloric acid and extracted with ethyl acetate. The ethyl acetate extract was washed with water and saturated sodium chloride solution, dried over anhydrous magnesium sulfate and evaporated to give an oil which soon crystallized. Trituration with petroleum yielded 1.92 g (35%) of N-benzyloxy 2(RS)-isobutyl-3-aminopropionic acid of melting point 73°-75° C. Rf (toluene/acetic acid 4:1) 0.52.

WORKUP

后处理

  1. customThe solvent was removed by evaporation
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washThe organic layer was washed with 2N hydrochloric acid and water
  4. extractionextracted six times with 30 ml of 5% sodium hydrogen carbonate solution each time
  5. extractionextracted with ethyl acetate
  6. extractionThe ethyl acetate extract
  7. washwas washed with water and saturated sodium chloride solution
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customevaporated
  10. customto give an oil which
  11. customsoon crystallized