HRID33416

反应详情

EQUATION

反应方程式

HRID 33416 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

From 7.6 g (0.33 mol) of sodium and 300 mL of ethanol, a sodium ethoxide solution is prepared, to which 69.6 g (0.33 mol) of 9-fluorenecarboxylic acid are added batchwise. After the addition has ended, the mixture is stirred for 2.5 hours at ambient temperature. Then it is evaporated to dryness, the residue is suspended in 600 mL of dimethylformamide, and 93.96 g (0.662 mol) of methyl iodide are added dropwise. The mixture is stirred for 3 hours at constant temperature. The cloudy solution is stirred into 500 mL of water and 300 mL of diethyl ether with cooling and extracted, the organic phase is washed with water and 10% sodium carbonate solution, dried, and evaporated to dryness. The residue is purified by column chromatography, eluent: cyclohexane-ethyl acetate (96:4). Yield: 12.61 g of white crystals (16% of theoretical yield); melting point: 108° C.-109° C.

WORKUP

后处理

  1. additionare added batchwise
  2. additionAfter the addition
  3. customThen it is evaporated to dryness
  4. stirringThe mixture is stirred for 3 hours at constant temperature
  5. temperaturewith cooling
  6. extractionextracted
  7. washthe organic phase is washed with water and 10% sodium carbonate solution
  8. customdried
  9. customevaporated to dryness
  10. customThe residue is purified by column chromatography, eluent