HRID626180

反应详情

EQUATION

反应方程式

HRID 626180 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of N-methoxy-N-methyl-1,4-dioxaspiro[4.5]decane-8-carboxamide (1 g, 0.0043 mol) in anhydrous Et2O (20 mL) was added EtMgBr (9 g, 0.043 mol). The reaction mixture was refluxed overnight, and then 200 mL water was added. The mixture was extracted with ethyl acetate. The extract was concentrated and purified by silica gel column chromatography (CH2Cl2:MeOH=150:1) to give the desired product (0.259 g, 26% yield).

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed overnight
  2. extractionThe mixture was extracted with ethyl acetate
  3. concentrationThe extract was concentrated
  4. custompurified by silica gel column chromatography (CH2Cl2:MeOH=150:1)