User:Elaine Marie Robbins/Notebook/MOF/2012/07/03

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Methods

  1. Pour reaction mixture into 20 mL of ice/concentrated HCl (3:1).
  2. Extract organic phase with chloroform (3x with 30 mL).
  3. Dry with 1 g magnesium sulfate.
  4. Remove magnesium sulfate with filter paper.
  5. Rotovap.
  6. At 20 mL toluene at 90°C to recrystallize.
  7. Allow to return to room temp.
  8. Place in ice.
  9. Filter out yellow crystals with nylon filter paper, no vacuum needed.
  10. Suspend 63.1 mg of crystals in 100 mL of THF/dioxane/water (ratio 5/2/2).
  11. Add 20 mL 2 M NaOH.
  12. Stir under reflux overnight at 85°C.