HRID2168198

反应详情

EQUATION

反应方程式

HRID 2168198 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. extractionthen extracted with DCM (3×100 ml)
  2. dry with materialThe organic layer was dried over anhydrous MgSO4
  3. concentrationconcentrated in vacuo to desired product
  4. customLCMS [MH+] 235@1.17 and 1.19 (isomers) (5 min run)