HRID235139

反应详情

EQUATION

反应方程式

HRID 235139 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 7-hydroxy-1-(4-methyl-1-piperazinyl)-naphthalene (0.065 g, 0.268 mmol) and benzoyl chloride (0.035 mL, 0.302 mmol) in methylene chloride (1 mL) and saturated sodium bicarbonate (1 mL) was stirred at room temperature. After several hours, a second equivalent of benzoyl chloride was added with continued stirring overnight. The reaction was diluted with ethyl acetate and the phases were separated. The organic layer was washed with 1N sodium hydroxide, water and brine; then it was dried over magnesium sulfate and concentrated to an oil which solidified (0.065 g, 69%). A sample recrystallized from ether/hexane as a light pink solid was submitted for analysis: mp 82°-82.5° C. Analysis calculated for C22H22N2O2 ·0.25 H2O: C, 75.30; H, 6.46; N, 7.98. Found: C, 75.51; H, 6.29; N, 7.97.

WORKUP

后处理

  1. waitAfter several hours
  2. stirringwith continued stirring overnight
  3. customthe phases were separated
  4. washThe organic layer was washed with 1N sodium hydroxide, water and brine
  5. dry with materialthen it was dried over magnesium sulfate
  6. concentrationconcentrated to an oil which
  7. customA sample recrystallized from ether/hexane as a light pink solid