HRID2187397
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethen cooled
- customthe excess TFA removed in vacuo
- additionThe residue was diluted with water
- extractionextracted with ether (3×)
- washAfter washing the ether layer with saturated NaHCO3
- dry with materialbrine, it was dried (Na2SO4)
- concentrationconcentrated
- customto give a viscous oil
- customPurification by silica gel chromatography (hexane:EtOAc 3:7)