HRID491910
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
A mixture of 3,3-dimethyl butylamine (0.6 mL, 4.2 mmol), 3-[benzyl-(1-phenyl-ethyl)-amino]-3-cyclohexyl-propionic acid (1.83 g, 3.8 mmol), HBTU (2.2 g, 5.7 mmol), DIPEA (1.5 mL, 8.6 mmol) and DMF (25 mL) was stirred at room temperature for 14 hours. To the reaction mixture was then added sodium bicarbonate(s) (100 mL) and the desired product was extracted with ethyl acetate (100 mL×2). The combined organic layers were washed with water, dried over MgSO4 and concentrated to yield a solid. The solid was purified by column chromatography (10% EtOAc/heptane) to yield a residue.
WORKUP
后处理
- extractionadded sodium bicarbonate(s) (100 mL) and the desired product was extracted with ethyl acetate (100 mL×2)
- washThe combined organic layers were washed with water
- dry with materialdried over MgSO4
- concentrationconcentrated
- customto yield a solid
- customThe solid was purified by column chromatography (10% EtOAc/heptane)
- customto yield a residue