HRID2187397

反应详情

EQUATION

反应方程式

HRID 2187397 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The ester 16-3 (5.7 g) in TFA (75 mL) was heated at 60° C. for 2 hours then cooled and the excess TFA removed in vacuo. The residue was diluted with water, made basic with NaHCO3 and extracted with ether (3×). After washing the ether layer with saturated NaHCO3 then brine, it was dried (Na2SO4) and concentrated to give a viscous oil. Purification by silica gel chromatography (hexane:EtOAc 3:7) afforded the title compound 16-4 as an oil.

WORKUP

后处理

  1. temperaturethen cooled
  2. customthe excess TFA removed in vacuo
  3. additionThe residue was diluted with water
  4. extractionextracted with ether (3×)
  5. washAfter washing the ether layer with saturated NaHCO3
  6. dry with materialbrine, it was dried (Na2SO4)
  7. concentrationconcentrated
  8. customto give a viscous oil
  9. customPurification by silica gel chromatography (hexane:EtOAc 3:7)