HRID36146
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 3.2 gms of the N-heptyl-N-ethylamine in 96 ml of CH2Cl2 are added 5.7 ml of Et3 followed by 3.63 ml of hexanedioic acid monochloride monomethyl ester. This mixture is stirred at room temperature for 18 hours; and after concentrating under vacuum, the residue obtained is partitioned between ethyl acetate and an aqueous 2N HCl solution. The organic layer is separated and washed with aqueous saturated NaHCO3, then brine, and dried over MgSO4. Following filtration and concentration under vacuum, the residue is flash chromatographed on normal phase silica gel using a 3/1 ratio of hexane and ethyl acetate to yield N-heptyl-N-ethyladipamic acid, methyl ester.
WORKUP
后处理
- concentrationand after concentrating under vacuum
- customthe residue obtained
- customis partitioned between ethyl acetate
- customThe organic layer is separated
- washwashed with aqueous saturated NaHCO3
- dry with materialbrine, and dried over MgSO4
- filtrationfiltration and concentration under vacuum
- customchromatographed on normal phase silica gel using a 3/1 ratio of hexane and ethyl acetate