HRID2168198
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 1,1-dimethylethyl 3-(methyloxy)-4-[(phenylcarbonyl)amino]-1-piperidinecarboxylate D20 (4.0 g) in HCl/1,4-dioxane (30 ml) was stirred at room temperature for overnight. The resulting mixture was dissolved in water (50 ml) and basified with sodium hydroxide to pH 10.0 then extracted with DCM (3×100 ml). The organic layer was dried over anhydrous MgSO4, concentrated in vacuo to desired product D21 as an oil in 500 mg. LCMS [MH+] 235@1.17 and 1.19 (isomers) (5 min run)
WORKUP
后处理
- extractionthen extracted with DCM (3×100 ml)
- dry with materialThe organic layer was dried over anhydrous MgSO4
- concentrationconcentrated in vacuo to desired product
- customLCMS [MH+] 235@1.17 and 1.19 (isomers) (5 min run)