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