HRID1420778

反应详情

EQUATION

反应方程式

HRID 1420778 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

3'-Amino-2'-hydroxyacetophenone (1.51 g, 10 mmol) was dissolved in 50 ml of acetone, and potassium carbonate (6.90 g, 50 mmol) was added to the solution. 4-(4-Phenylbutoxy)benzoyl chloride (2.89 g, 10 mmol) was added dropwise to the mixture under stirring at 0° C., and stirring was conducted further for 3 hours. The resultant reaction mixture was poured into a 10% hydrochloric acid (100 ml) to conduct extraction with chloroform. An organic layer was washed with water, dried and then concentrated under reduced pressure. The residue was subjected to column chromatography on silica gel. Crystals obtained from a fraction eluted with chloroform were recrystallized from ethanol to obtain 2.82 g (yield: 70%) of 2-hydroxy-3-[4-(4-phenylbutoxy)benzamido)]acetophenone.

WORKUP

后处理

  1. stirringstirring
  2. customThe resultant reaction mixture
  3. extractionextraction with chloroform
  4. washAn organic layer was washed with water
  5. customdried
  6. concentrationconcentrated under reduced pressure
  7. customCrystals obtained from a fraction
  8. washeluted with chloroform
  9. customwere recrystallized from ethanol