HRID2428202
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
- 70 °C
PROCEDURE
实验过程
A mixture of compound C8 (1.00 g, 1.78 mmol) and aq. 1M LiOH (7.00 mL, 7.00 mmol) in THF (7.00 mL) was stirred overnight at 70° C. Aq. 1M HCl was added until a pH=4 was reached. The mixture was extracted with EtOAc (3×). The combined org. extracts were dried over MgSO4, filtered, and the solvents were removed under reduced pressure. Drying the residue under high vacuum yielded the title compound mixed with 6-[3-(2-chloro-3,6-difluoro-phenyl)-isoxazol-5-ylmethoxy]-3′,6′-dihydro-2′H-[3,4′]bipyridinyl-1′,3′-dicarboxylic acid 1′-tert-butyl ester (976 mg, quantitative yield) that was used further without purification. LC-MS: tR=1.06 min; ES+: 548.30.
WORKUP
后处理
- extractionThe mixture was extracted with EtOAc (3×)
- dry with materialextracts were dried over MgSO4
- filtrationfiltered
- customthe solvents were removed under reduced pressure
- customDrying the residue under high vacuum