HRID1942303
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 solution of lithium hydroxide (19.7 mg, 0.822 mmol) in water (1 ml) was added to a stirred solution of the ester (Step 3, 96 mg, 0.164 mmol) in THF (2 ml) at RT. The mixture was stirred at RT o/n. 2N HCl (1 ml) was added The pH of the aqueous layer was adjusted to 7 with NaHCO3 (aq). The aqueous layer was extracted with DCM (×3). The combined extracts were dried (Na2SO4), filtered and evaporated. The residue was purified by chromatography (silica, 2-5% MeOH/DCM) to give the acid (91 mg) as a colourless oil. M/Z 570 (MH+).
WORKUP
后处理
- extractionThe aqueous layer was extracted with DCM (×3)
- dry with materialThe combined extracts were dried (Na2SO4)
- filtrationfiltered
- customevaporated
- customThe residue was purified by chromatography (silica, 2-5% MeOH/DCM)