HRID1865253
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
6 N HCl (200 ml) was added to a stirred solution of 4-benzyloxycarbonylamino-1-t-butyloxycarbonyl-3,3-dimethylpiperidine (350 g, 0.96 mol) in dioxane (200 ml). The resulting mixture was stirred for 1 hr and concentrated to dryness. The resultant residue was treated with water (3.0 L) water and was extracted with 1.0 L×2 ethyl acetate. The aqueous layer was basified with 2 M aqueous NaOH and extracted with 2.5 L×2 dichloromethane. Combined organic extract was washed with water, dried over Na2SO4 and concentrated to afford 4-benzyloxycarbonylamino-3,3-dimethylpiperidine in 89% (224 g) yield.
WORKUP
后处理
- concentrationconcentrated to dryness
- additionThe resultant residue was treated with water (3.0 L) water
- extractionwas extracted with 1.0 L×2 ethyl acetate
- extractionextracted with 2.5 L×2 dichloromethane
- extractionCombined organic extract
- washwas washed with water
- dry with materialdried over Na2SO4
- concentrationconcentrated