HRID1700175
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
2-Fluoro-4-(3-methyl-4,5,6,7-tetrahydro-3H-imidazo[4,5-c]pyridin-4-yl)-benzonitrile (Step E) (0.034 g, 0.132 mmol), 3-(3-methoxy-benzenesulfonylamino)-propionic acid (Step G) 0.041 g, 0.16 mmol), HOBT (0.022 g, 0.16 mmol), EDC (0.031 g, 0.16 mmol) and N-methylmorpholine (0.043 mL, 0.40 mmol) were dissolved in DMF (3 mL) and stirred for 18 h. The reaction mixture was concentrated in vacuo, diluted with CH2Cl2 and saturated NaHCO3 solution and separated. The aqueous layer was washed with CH2Cl2 (2×, the organic layers combined, dried (Na2SO4), filtered and concentrated to give the title compound.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated in vacuo
- additiondiluted with CH2Cl2 and saturated NaHCO3 solution
- customseparated
- washThe aqueous layer was washed with CH2Cl2 (2×
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated