HRID967409

反应详情

EQUATION

反应方程式

HRID 967409 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-(2-Ethoxycarbonylmethoxy-phenylamino)-piperidine-1-carboxylic acid tert-butyl ester (21.4 g, 56.5 mmol) was set stirring in MeOH (150 mL). A solution of NaOH (4.5 g, 112.5 mmol) in water (150 mL) was added. After 3 h the mixture was acidified to pH 4 with 6 N HCl. MeOH was removed under reduced pressure and the aqueous layer extracted with EtOAc (2×150 mL). The organics were combined, dried (MgSO4) and evaporated to give 20 g (100%) of a brown solid. MS (electrospray): exact mass calculated for C18H26N2O5, 350.18. m/z found, 351.2 [M+H]+.

WORKUP

后处理

  1. customMeOH was removed under reduced pressure
  2. extractionthe aqueous layer extracted with EtOAc (2×150 mL)
  3. dry with materialdried (MgSO4)
  4. customevaporated