HRID17896

反应详情

EQUATION

反应方程式

HRID 17896 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-Phenyl-6-(3-phenylpropyloxy)-1-oxo-1H-indene-2-carboxylate ethyl ester (1.65 g, 4.0 mmol) prepared in (Step 5) of Example 1 was dissolved in methanol (160 ml) and p-toluene sulfonic acid (228 mg, 1.2 mmol) was added thereto. The mixture was reacted for 1 hour at 70° C., and then washed with brine. The organic layer was extracted with ethyl acetate, dried over anhydrous sulfonate sulfate, concentrated, and the resulting residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:9) to obtain the title compound (yield 75.3%) as a red solid.

WORKUP

后处理

  1. customThe mixture was reacted for 1 hour at 70° C.
  2. washwashed with brine
  3. extractionThe organic layer was extracted with ethyl acetate
  4. dry with materialdried over anhydrous sulfonate sulfate
  5. concentrationconcentrated
  6. customthe resulting residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:9)