HRID1731036

反应详情

EQUATION

反应方程式

HRID 1731036 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution containing 2.4 mmol. of phenyl lithium in benzene-ether was added dropwise at -78° under argon to a solution of 700 mg. (2.4 mmol.) of N-t-butoxycarbonyl-2-acetoxyglycine n-butyl ester in 15 ml. of dry ether. The mixture was stirred for 2 hours at -78°, then for 1 hour at 25°. The mixture was diluted with water, the layers were separated and the ether layer was washed with water, dried (Na2SO4) and concentrated in vacuo. The residue was chromatographed on silica gel with methylene chloride to give a crude product which was rechromatographed on basic alumina to give the title compound.

WORKUP

后处理

  1. additionA solution containing 2.4 mmol
  2. waitfor 1 hour at 25°
  3. customthe layers were separated
  4. washthe ether layer was washed with water
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated in vacuo
  7. customThe residue was chromatographed on silica gel with methylene chloride
  8. customto give a crude product which
  9. customwas rechromatographed on basic alumina