HRID1672732
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 4,4-difluoro-cyclohexylamine (295 mg) and Et3N (0.91 mL) in 22 mL of CH2Cl2, add 4-chloro-butyryl chloride (0.42 g). Allow the resulting mixture to stand at room temp for 4 hr. Remove the organic solvent under vacuum. Dissolve the residue in Et2O. Wash the organic layer with 1N HCl, then brine, and then H2O, and dry over Na2SO4, filter and concentrate. Purify the crude material by chromatography to afford 0.41 g of the title compound: mass spectrum (m/z): 240 (M+1).
WORKUP
后处理
- customRemove the organic solvent under vacuum
- dissolutionDissolve the residue in Et2O
- washWash the organic layer with 1N HCl
- dry with materialbrine, and then H2O, and dry over Na2SO4
- filtrationfilter
- concentrationconcentrate
- customPurify the crude material by chromatography