HRID2069873

反应详情

EQUATION

反应方程式

HRID 2069873 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2,6-Dibromophenol (29.30 g, 116 mmol) and benzyl bromide (33.14 g, 194 mmol) were dissolved in 2-butanone (300 mL). Potassium carbonate (29.47 g, 213 mmol) was added, and the mixture was stirred for 1.5 hr at reflux temperature. The reaction mixture was cooled to room temperature, filtered, and evaporated to dryness. The remaining viscous oil was subjected to silicagel column chromatography, flushing with n-pentane to remove benzyl bromide, then DCM/n-pentane=1:1 to elute the product, yielding the product as a white crystalline solid (39.32 g, 99%). 1H-NMR (CDCl3): δ=7.61 (dd, 2H), 7.54 (d, 2H), 7.41 (m, 3H), 6.90 (t, 1H), 5.04, (s, 2H) ppm.

WORKUP

后处理

  1. temperatureat reflux temperature
  2. filtrationfiltered
  3. customevaporated to dryness
  4. customflushing with n-pentane
  5. customto remove benzyl bromide
  6. washDCM/n-pentane=1:1 to elute the product