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 Trans-2-amino-1-cyclohexane carboxylic acid (100 mg, 0.7 mmol) in 1 mL of water is added 2M aqueous Na2CO3 until pH=9-10 (2 mL). A solution of the carbonic acid 4-nitro-phenyl ester thiophen-2-ylmethyl ester (195 mg, 0.7 mmol) in THF (1 mL) is added at 0° C. and, after 10 minutes, 1 ml of the 2M Na2CO3 is added to the reaction. The mixture is allowed to warm to RT and vigorously stirred overnight. The reaction mixture is diluted with 0.5N HCl until pH=4-3 and the water layer is extracted three times with CH2Cl2 (10 ml). The organic phases are combined, dried (MgSO4), and concentrated under reduced pressure. The resulting product is used in the next step without further purification.
WORKUP
后处理
- extractionthe water layer is extracted three times with CH2Cl2 (10 ml)
- dry with materialdried (MgSO4)
- concentrationconcentrated under reduced pressure
- customThe resulting product is used in the next step without further purification