HRID895712

反应详情

EQUATION

反应方程式

HRID 895712 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The compound (t-butyl 2-fluoro-5-nitrobenzoate) (1.74 g) obtained in a previous production example, 6-cyano-2-naphthol (1.86 g) and potassium carbonate (8.2 g) were heated to 50° C. in N,N-dimethylformamide and reacted for 2 hours. After cooling to room temperature, water was added and extraction was performed with ethyl acetate. The ethyl acetate layer was washed with saturated saline and dried over magnesium sulfate, and the solvent was distilled off. The residue was purified by silica gel chromatography (300 g, hexane:ethyl acetate=5:1) to obtain 3.23 g of t-butyl 2-(6-cyano-2-naphthyloxy)-5-nitrobenzoate.

WORKUP

后处理

  1. customreacted for 2 hours
  2. extractionextraction
  3. washThe ethyl acetate layer was washed with saturated saline
  4. dry with materialdried over magnesium sulfate
  5. distillationthe solvent was distilled off
  6. customThe residue was purified by silica gel chromatography (300 g, hexane:ethyl acetate=5:1)