HRID919595
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 tert-butyl(S)-1-(2-(3,5-dichlorophenylamino)acetyl)piperidin-3-ylcarbamate (0.9 mg, 2.2 mmol) in 1,4-dioxane (5 mL) was added 4 N HCl in dioxane (10 mL) and the reaction mixture was stirred for 1 h. The reaction mixture was concentrated in vacuo and the resultant residue was dissolved in water and aqueous phase was adjusted to a pH 9 with sat. NaHCO3 and extracted with EtOAc (3×50 mL). The combined organic layer was dried over Na2SO4 and evaporated in vacuo to afford the titled intermediate (540 mg, 79%), which was used in the next step without purification. LCMS: m/z: [M+1]=302.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated in vacuo
- dissolutionthe resultant residue was dissolved in water
- extractionextracted with EtOAc (3×50 mL)
- dry with materialThe combined organic layer was dried over Na2SO4
- customevaporated in vacuo