HRID1896854

反应详情

EQUATION

反应方程式

HRID 1896854 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of sodium hydride (27 mg, 1.07 mmol, 95%) in THF under argon was added 5-(1,4-dioxaspiro[4.5]decan-8-yl)pyrrolidin-2-one (135 mg, 0.60 mmol, prepared in the Example 12 Step E). After stirring 1 hour at room temperature, Methyl iodide (0.07 mL, 1.12 mmol) was added dropwise and the reaction stirred at room temperature overnight. The reaction mixture was poured onto saturated NaHCO3 and extracted with ethyl acetate. The organic layer was concentrated in vacuo and the residue purified by flash chromatography (silica gel, 0-100% ethyl acetate/DCM).

WORKUP

后处理

  1. customprepared in the Example 12 Step E)
  2. stirringthe reaction stirred at room temperature overnight
  3. extractionextracted with ethyl acetate
  4. concentrationThe organic layer was concentrated in vacuo
  5. customthe residue purified by flash chromatography (silica gel, 0-100% ethyl acetate/DCM)