HRID1868696
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
CONDITIONS
反应条件
- 温度
- 130 °C
PROCEDURE
实验过程
A flask containing a solution of methyl 2-(2-fluorophenyl)-2-methylpropanoate (5.2 g, 27 mmol), KOH (2.9 mL, 106 mmol), water (20.0 mL), and EtOH (100 mL) was sealed and heated at 130° C. for 2 hours. Removal of solvent in vacuo provided a yellow oil that was diluted with water. The aqueous mixture was extracted with DCM (1×100 mL), and the organic layer was separated. The aqueous layer was acidified to a pH of 1 with 5N HCl and then extracted with EtOAc (2×100 mL). The organic layers were dried (Na2SO4), filtered, and concentrated in vacuo to afford 4 g of the product as a solid. MS (m/z)=181 (M−1)−.
WORKUP
后处理
- customwas sealed
- customRemoval of solvent in vacuo
- customprovided a yellow oil that
- extractionThe aqueous mixture was extracted with DCM (1×100 mL)
- customthe organic layer was separated
- extractionextracted with EtOAc (2×100 mL)
- dry with materialThe organic layers were dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated in vacuo