HRID1680508

反应详情

EQUATION

反应方程式

HRID 1680508 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

A mixture of 1,3-dihydro-3-(1-nitroethyl)-isobenzofuran-1-one [2.0 g, described by J. J. Stehle et al., J. Org. Chem., 10, 429 (1945)], dimethyl sulfate (1.6 ml) and potassium carbonate (2.4 g) in acetone (50 ml) is stirred at 25° C. for 18 hr under dry conditions. The mixture is filtered and the filtrate is evaporated. The residue is chromatographed on silica gel using benzene and the eluates are evaporated to give the title compound (1.672 g), nmr (CDCl3) δ2.25(s), 3.91(s), 7.40(s), 7.60(m), 8.18(s) and 8.50(s).

WORKUP

后处理

  1. filtrationThe mixture is filtered
  2. customthe filtrate is evaporated
  3. customThe residue is chromatographed on silica gel
  4. customthe eluates are evaporated