HRID377198

反应详情

EQUATION

反应方程式

HRID 377198 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

2-Piperidine ethanol (39.6 ml, 0.31 mol) was dissolved in 5M aq NaOH (62 ml, 0.31 mol) and dioxan (100 ml). The mixture was cooled to 0° C. and treated with benzyl chloroformate (45.3 ml, 0.32 mol) and 5M NaOH (62 ml, 0.31 mol). Stirring was continued at room temp. for 18 hours. Dioxan was removed in vacuo and the aqueous phase extracted with ether before acidifying with 5N HCl and extracting again with ether. The organic phase was dried and evaporated in vacuo and the residue purified by chromatography on silica gel to give the title compound (77.2 g. 95%). MH+ 264.

WORKUP

后处理

  1. customDioxan was removed in vacuo
  2. extractionthe aqueous phase extracted with ether
  3. extractionextracting again with ether
  4. customThe organic phase was dried
  5. customevaporated in vacuo
  6. customthe residue purified by chromatography on silica gel