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
- 0 °C
PROCEDURE
实验过程
A solution of 4-fluorobenzoyl chloride (0.113 mL, 0.957 mmol) in DCM (2.90 mL) was cooled to 0° C. under nitrogen. To this was added cis-methyl 4-(2-amino-6-((triisopropylsilyloxy)methyl)-1H-benzo[d]imidazol-1-yl)cyclohexanecarboxylate (0.4 g, 0.870 mmol) followed by TEA (0.482 mL, 3.48 mmol). The resulting mixture was stirred at 0° C. for 30 minutes. The ice bath was removed, and the mixture was stirred for 2 hours. The reaction mixture was diluted with DCM (20 mL) and washed with water (10 mL). The organic layer was collected, dried over sodium sulfate, concentrated, and dried under vacuum to afford cis-methyl 4-(2-(4-fluorobenzamido)-6-((triisopropylsilyloxy)methyl)-1H-benzo[d]imidazol-1-yl)cyclohexanecarboxylate (0.5 g, 100% yield).
WORKUP
后处理
- customThe ice bath was removed
- stirringthe mixture was stirred for 2 hours
- additionThe reaction mixture was diluted with DCM (20 mL)
- washwashed with water (10 mL)
- customThe organic layer was collected
- dry with materialdried over sodium sulfate
- concentrationconcentrated
- customdried under vacuum