HRID1068578

反应详情

EQUATION

反应方程式

HRID 1068578 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 the 6-(3,4-dimethoxyphenyl)-3,4,5,6-tetrahydro-2H-1,3-oxazin-2-one (1.20 g, 5.06 mM) produced in Example 1 in dried N,N-dimethylformamide (30 ml) were added sodium hydride (60%) (0.41 g, 10.12 mM) and methyl iodide (1.44 g, 10.12 mM). The solution was then stirred at room temperature for one night. The reaction solution was carefully poured into ice water, then extracted with methylene chloride. The extract was dried over anhydrous sodium sulfate and the solvent was removed in vacuo to obtain a residue as a brown oil. The residue was purified by flash chromatography (SiO2; eluted by 0.5% methanol/chloroform) to obtain the above-described compound 0.28 g (yield 22.3%) as a colorless solid.

WORKUP

后处理

  1. extractionextracted with methylene chloride
  2. dry with materialThe extract was dried over anhydrous sodium sulfate
  3. customthe solvent was removed in vacuo