HRID1743641

反应详情

EQUATION

反应方程式

HRID 1743641 的结构方程式

PROCEDURE

实验过程

A 10.0 g of 9-fluorenone-4-carbonyl chloride (0.04 mole, obtained from Aldrich Chemicals Co, Milwaukee, Wis. 53201, USA) and 100 ml of tetrahydrofuran (obtained from Aldrich) were added to a 250 ml, 3-neck round bottom flask equipped with a reflux condenser and a mechanical stirrer. The solution was stirred for about ½ hour, then 5.16 g of 4,4′-thiobisbenzenethiol (0.02 mole, obtained from Aldrich) in 50 ml of tetrahydrofuran were added, followed by the addition of 4.17 g of triethylamine (0.04 mole, obtained from Aldrich). The solution was refluxed for 6 hours and filtered hot to remove triethylamine hydrochloride salt byproduct. The filtrate was evaporated to dryness to obtain the crude product. The crude product was recrystallized from tetrahydrofuran/methanol with activated charcoal. The product was dried at 60° C. vacuum oven for 6 hours to yield a first dimeric fluorenone derivative, which was a yellow solid (6.85 g, 50% yield).

WORKUP

后处理

  1. customequipped with a reflux condenser and a mechanical stirrer
  2. temperatureThe solution was refluxed for 6 hours
  3. filtrationfiltered hot
  4. customto remove triethylamine hydrochloride salt byproduct
  5. customThe filtrate was evaporated to dryness
  6. customto obtain the crude product
  7. customThe crude product was recrystallized from tetrahydrofuran/methanol with activated charcoal
  8. customThe product was dried at 60° C. vacuum oven for 6 hours