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
Ethyl 2-methyl-2-({2-methyl-4-[(1-{6-[4-(trifluoromethyl)phenyl]-2-pyridinyl}pentyl)oxy]phenyl}oxy)propanoate (9 mg, 0.02 mmol) was dissolved in THF (0.75 mL), water (0.25 mL) and aqueous NaOH (2M, 35 μl, 0.07 mmol) and the mixture heated at 80° C. for 16 hours. More aqueous NaOH (2M, 420 μl, 0.84 mmol) was then added and heating continued for an additional 24 hours. The mixture was then cooled, neutralised with aqueous HCl (2M), partitioned between EtOAc and water and the layers separated. The organic layer was then washed with brine, dried (Na2SO4) and reduced to give a pale yellow oil. Purification by SPE (aminopropyl, 1 g cartridge) loading in CHCl3 and eluting with dioxane and then 10% aqueous ammonia in dioxane afforded the title compound as a colourless gum (4.5 mg).
WORKUP
后处理
- temperatureheating
- temperatureThe mixture was then cooled
- custompartitioned between EtOAc and water
- customthe layers separated
- washThe organic layer was then washed with brine
- dry with materialdried (Na2SO4)
- customto give a pale yellow oil
- customPurification by SPE (aminopropyl, 1 g cartridge) loading in CHCl3
- washeluting with dioxane