HRID591559
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of anisole (12.04 g), 1-fluoro-3-methoxy-5-((4-methoxybenzyl)sulfanyl)benzene (6.2 g) and TFA (20 mL) was refluxed for 1 h, then concentrated in vacuo. Water was added to the residue and the mixture was extracted with EtOAc. The organic layer was washed with saturated aqueous NaHCO3 and extracted with 2N NaOH (100 mL×3). The water layer was acidified with 6N HCl and extracted with EtOAc. The EtOAc extract was washed successively with water and brine, dried over MgSO4, and concentrated in vacuo to give the title compound (2.30 g).
WORKUP
后处理
- temperaturewas refluxed for 1 h
- concentrationconcentrated in vacuo
- additionWater was added to the residue
- extractionthe mixture was extracted with EtOAc
- washThe organic layer was washed with saturated aqueous NaHCO3
- extractionextracted with 2N NaOH (100 mL×3)
- extractionextracted with EtOAc
- extractionThe EtOAc extract
- washwas washed successively with water and brine
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo