HRID1677071

反应详情

EQUATION

反应方程式

HRID 1677071 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Under a nitrogen atmosphere, 4-chlorophenyl magnesium bromide (64.1 mL, 1 M tetrahydrofuran solution) was added dropwise at −40° C. into a tetrahydrofuran (300 mL) solution of (R)-5-oxopyrrolidine-1,2-dicarboxylic acid 1-t-butyl ester 2-ethyl ester (15 g) obtained in Example 4. After stirring for 1 hour at the same temperature, saturated ammonium chloride aqueous solution was added, and extraction with ethyl acetate was conducted. After washing the organic layer with brine, the resultant was dried over anhydrous magnesium sulfate. The solvent was removed under a vacuum, and the residue was purified by silica gel column chromatography (heptane→heptane/ethyl acetate), and the title compound (17.38 g) was obtained. The physical property values are as follows.

WORKUP

后处理

  1. additionwas added
  2. extractionextraction with ethyl acetate
  3. washAfter washing the organic layer with brine
  4. dry with materialthe resultant was dried over anhydrous magnesium sulfate
  5. customThe solvent was removed under a vacuum
  6. customthe residue was purified by silica gel column chromatography (heptane→heptane/ethyl acetate)