HRID506848

反应详情

EQUATION

反应方程式

HRID 506848 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 3-bromo-4-fluorobenzaldehyde (5.0 g, 24.6 mmol) in H2SO4 (25 mL) at 0° C. was added nitric acid (3 mL) in H2SO4 (30 mL), dropwise. The resulting mixture was warmed to room temperature overnight. The resulting solution was then poured slowly over ice and filtered to collect the yellow precipitate. The precipitate was washed with H2O and dried, then purified by silica gel chromatography eluted with a solvent mixture of ethyl acetate and heptanes from 0:100 to 25:75 to yield a light yellow solid.

WORKUP

后处理

  1. additionThe resulting solution was then poured slowly over ice
  2. filtrationfiltered
  3. customto collect the yellow precipitate
  4. washThe precipitate was washed with H2O
  5. customdried
  6. custompurified by silica gel chromatography
  7. washeluted with a solvent mixture of ethyl acetate and heptanes from 0:100 to 25:75
  8. customto yield a light yellow solid