HRID1614723

反应详情

EQUATION

反应方程式

HRID 1614723 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.37 g of 1,2,4-trihydroxy benzene and 30 ml of anhydrous dimethylformamide were mixed together under an inert gas atmosphere and then 0.984 g of sodium hydride in suspension at 53% in oil was added at 15°-20° C. The mixture was stirred for one hour and 1.906 ml of triethyl borate were added. The mixture was stirred for one hour, and 1.29 ml of benzyl bromide in solution in 20 ml of dimethylformamide were added over 2 hours. The mixture was stirred for 16 hours at ambient temperature and then was poured into a water-ice-N hydrochloric acid mixture. Extraction took place with ethyl acetate followed by evaporation to dryness. The residue was washed with petroleum ether, and chromatographed on silica eluting with a cyclohexane-ethyl acetate (6-4) mixture to obtain 1.36 g of the crystallized expected product (Yield: 58%).

WORKUP

后处理

  1. stirringThe mixture was stirred for one hour
  2. stirringThe mixture was stirred for 16 hours at ambient temperature
  3. extractionExtraction
  4. customfollowed by evaporation to dryness
  5. washThe residue was washed with petroleum ether
  6. customchromatographed on silica eluting with a cyclohexane-ethyl acetate (6-4) mixture
  7. customto obtain 1.36 g of the