tags
sodiumCO2chloroformdistillatehydrogenChloroformchlorotrichloroaceticcarbontrichloroacetatesodium saltcalcium

video tutorial An unusual preparation of chloroform

  • Overview: Converted trichloroacetic acid to chloroform via thermal decarboxylation of the formed sodium trichloroacetate in aqueous solution.
  • Starting materials and setup: 80 g trichloroacetic acid dissolved in water (initially 100 mL, final ~150 mL). 10 g NaOH added to neutralize about half, forming the sodium salt; reaction is exothermic.
  • Reaction conditions: 500 mL two‑neck flask with heating mantle, thermometer, Liebig condenser, and receiving flask; ice-cold water in condenser to maximize chloroform yield.
  • Process observations: Distillation at ~90–98 C; CO2 evolution; formation of two liquid layers; distillate collected over ~2 hours; final solution alkaline due to NaOH/Na2CO3 formation.
  • Product isolation and yield: Distillate separated; crude product ~24 mL (36 g) with the classic chloroform aroma; dried with anhydrous CaCl2; stored in a pre‑weighed bottle; yield ~58% of theoretical maximum; remainder likely remained in flask or evaporated.
  • Notes: The reaction is faster with the sodium salt present; considered an interesting, relaxing experiment; previous video on reducing TCAA to DCAA with zinc.

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