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
- 100 °C
PROCEDURE
实验过程
To a solution of tert-Butyl (3R,4S)-3-({cyclopropyl[3-(4-methoxy-3,3-dimethyl-4-oxobutoxy)-5-(3-methoxypropyl)-benzyl]amino}carbonyl)-4-{4-[2-(2,6-dichloro-4-methylphenoxy)ethoxy]phenyl}-piperidine-1-carboxylate (1 eq.) from Example 21/Step 2 in ethanol was added 1 N aqueous NaOH (3 eq.). The reaction was heated to 100° C. for 10 min in a microwave reactor (Biotage). After cooling to rt, the reaction was concentrated in vacuo to removed the ethanol solvent. The resulting solution was acidified with 1 N HCl and extracted with ethyl acetate. The combined organic extracted were dried over anhydrous Na2SO4 and concentrated in vacuo. The crude product was used in the next step without further purification.
WORKUP
后处理
- temperatureAfter cooling to rt
- concentrationthe reaction was concentrated in vacuo
- customto removed the ethanol solvent
- extractionextracted with ethyl acetate
- extractionThe combined organic extracted
- dry with materialwere dried over anhydrous Na2SO4
- concentrationconcentrated in vacuo
- customThe crude product was used in the next step without further purification