HRID2059894
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
Methyl 4-(1-(4-methoxy-2,6-dimethylphenylsulfonyl)piperidin-2-yl)butanoic acid methyl ester (1.65 g, 4.3 mmol) was dissolved in water (10 ml) and methanol (35 ml) and lithium hydroxide (0.3 g, 12.9 mmol) was added. The mixture was stirred for 3 d at room temperature, then methanol was distilled off under vacuum and ethyl acetate (50 ml) and HCl solution (1 mol/l, 10 ml) added to the residue. Phase separation, extraction with ethyl acetate (2×50 ml), the combined organic phases were dried over sodium sulfate and concentrated to small volume under vacuum. Yield: 1.56 g (98%)
WORKUP
后处理
- distillationmethanol was distilled off under vacuum and ethyl acetate (50 ml) and HCl solution (1 mol/l, 10 ml)
- additionadded to the residue
- customPhase separation, extraction with ethyl acetate (2×50 ml)
- dry with materialthe combined organic phases were dried over sodium sulfate
- concentrationconcentrated to small volume under vacuum