HRID485649

反应详情

EQUATION

反应方程式

HRID 485649 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Fifty grams of 2,4-dihydroxyacetophenone were dissolved in 250 ml. of dimethylformamide and the solution was cooled to 0° C. by means of an external ice-bath. After the addition of 15 grams of a 50% oil dispersion of sodium hydride, 40 ml. of benzyl chloride were added in a dropwise fashion and the reaction was allowed to warm to room temperature. After stirring overnight, the reaction mixture was added to 700 ml. of ethyl acetate. The organic phase was washed with 1000 ml. of 1N hydrochloric acid and twice each with 1000 ml. of a saturated sodium chloride solution. The organic layer was dried, and the solvent removed in vacuo. The oily residue was treated with 100 ml. of methanol and 50 ml. of hexane. The desired 2-hydroxy-4-benzyloxyacetophenone (36.7 grams) was recovered by filtration.

WORKUP

后处理

  1. additionthe reaction mixture was added to 700 ml
  2. washThe organic phase was washed with 1000 ml
  3. customThe organic layer was dried
  4. customthe solvent removed in vacuo
  5. additionThe oily residue was treated with 100 ml
  6. filtrationThe desired 2-hydroxy-4-benzyloxyacetophenone (36.7 grams) was recovered by filtration