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
To a solution of cis-methyl 4-((E)-2-(4-fluorobenzoylimino)-6-((4-(2-hydroxypropan-2-yl)piperidin-1-yl)methyl)-2,3-dihydro-1H-benzo[d]imidazol-1-yl)cyclohexanecarboxylate (1.05 g, 1.907 mmol) in MeOH (20 mL) was added 1 N aqueous NaOH (19.07 mL, 19.07 mmol). The solution was stirred overnight at RT. After 2 days, the reaction solution was concentrated, the pH was adjusted to 4 with 2 N aqueous HCl, and the mixture was extracted with 9:1 DCM/2-propanol. The organic layer was dried over anhydrous magnesium sulfate, filtered, and concentrated to generate cis-4-((E)-2-(4-fluorobenzoylimino)-6-((4-(2-hydroxypropan-2-yl)piperidin-1-yl)methyl)-2,3-dihydro-1H-benzo[d]imidazol-1-yl)cyclohexanecarboxylic acid (1.01 g, 1.882 mmol, 99% yield) as a white powder. MS, m/z (C30H37PN4O4): calcd, 536.3. found, 537.0 [M+H].
WORKUP
后处理
- waitAfter 2 days
- concentrationthe reaction solution was concentrated
- extractionthe mixture was extracted with 9:1 DCM/2-propanol
- dry with materialThe organic layer was dried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationconcentrated