HRID16379

反应详情

EQUATION

反应方程式

HRID 16379 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-nitrobenzoic acid (S)-1-[(3R,5R)-5-(4-chlorophenyl)morpholine-3-yl]ethyl ester (1.46 g mg) in methanol (40 mL) was added sodium methoxide (1.9 mL, 28% methanol solution), and the resultant solution was stirred at room temperature for 1 hour. Solvent was removed by distillation under reduced pressure, and the resultant product was diluted with ethyl acetate and water. The organic layer was partitioned and washed with brine. The organic layer was then dried over anhydrous magnesium sulfate. Solvent was removed by distillation under reduced pressure, and the resulting residue was purified by silica gel column chromatography (heptane/ethyl acetate 9/1→1/3), to thereby obtain the titled compound (833 mg). The physical properties of the compound were as follows.

WORKUP

后处理

  1. customSolvent was removed by distillation under reduced pressure
  2. additionthe resultant product was diluted with ethyl acetate and water
  3. customThe organic layer was partitioned
  4. washwashed with brine
  5. dry with materialThe organic layer was then dried over anhydrous magnesium sulfate
  6. customSolvent was removed by distillation under reduced pressure
  7. customthe resulting residue was purified by silica gel column chromatography (heptane/ethyl acetate 9/1→1/3)