HRID455909
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
3.90 g potassium carbonate and 1.30 ml methyl iodide are added to 4.65 g 1-tert.-butoxycarbonylamino-4-oxo-cyclohexanecarboxylic acid in 45 ml N,N-dimethylformamide and the reaction mixture is stirred for three hours at ambient temperature. Then the solvent is distilled off using the rotary evaporator and the residue is divided between 10% potassium carbonate solution and diethyl ether. The aqueous phase is separated off and extracted with diethyl ether and the combined organic phases are washed with saturated sodium chloride solution, dried on magnesium sulphate and evaporated down. A colourless oil is left, which slowly crystallises.
WORKUP
后处理
- distillationThen the solvent is distilled off
- customthe rotary evaporator
- customThe aqueous phase is separated off
- extractionextracted with diethyl ether
- washthe combined organic phases are washed with saturated sodium chloride solution
- customdried on magnesium sulphate
- customevaporated down
- waitA colourless oil is left
- customwhich slowly crystallises