HRID895714

反应详情

EQUATION

反应方程式

HRID 895714 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The compound (4-(6-cyano-2-naphthyloxy)-3-(2-formylphenyl)nitrobenzene) (800 mg) obtained in a previous production example, 2-methyl-2-butene (1.4 ml) and sodium dihydrogen phosphate dihydrate (2 g) were dissolved in acetonitrile:water (2:1, 50 ml) and then sodium chlorate (1 g) was added. After reaction for one hour at room temperature, 1 N hydrochloric acid water was added and extraction was performed with ethyl acetate. The ethyl acetate layer was washed with 1N hydrochloric acid water and saturated saline and then dried over magnesium sulfate, and the solvent was distilled off to obtain 5′-nitro-2′-(6-cyano-2-naphthyloxy)-1,1′-biphenyl-2-carboxylic acid (800 mg). This was dissolved in toluene without purification and subjected to the same process as in Production Example 1 to obtain t-butyl 2′-(6-cyano-2-naphthyloxy)-5′-nitro-1,1′-biphenyl-2-carboxylate.

WORKUP

后处理

  1. customAfter reaction for one hour at room temperature
  2. extractionextraction
  3. washThe ethyl acetate layer was washed with 1N hydrochloric acid water and saturated saline
  4. dry with materialdried over magnesium sulfate
  5. distillationthe solvent was distilled off