Sodium Hydroxide → HCID 12799746, compound

Participants

Reaction Conditions

Reaction Steps

Into a 150 milliliter, 3-neck flask equipped with a Claisen adaptor, paddle stirrer, thermometer, addition funnel and condenser were charged 7.1 grams (0.060 mole) of 2-methyl-2-methoxypropanoic acid, prepared above, (5.5 grams, 0.060 mole) of thiosemicarbazide and 50 milliliters of dry dioxane. The slurry was heated to 85° C. and the addition funnel was charged with phosphorous oxychloride (POCl3). The POCl3 (10.1 grams, 0.066 mole) was slowly added (for 20 minutes) while maintaining the temperature within 85°-95° C. The resulting suspension was refluxed for 1 hour and topped slightly with a water aspirator and then cooled. Fifty (50) milliliters of water was added and 50% solution of NaOH was also added until the pH of the solution was 10; an aqueous phase formed. The mixture was placed in a continuous diethylether extractor and extracted for 16 hours.

Provenance & Evidence