A mixture of 10 g (0.11 mole) of thiosemicarbazide and 70 ml of pyridine was prepared in a 250-ml four-necked round-bottomed flask fitted with mercury-sealed stirrer, dropping funnel, calcium chloride tube, and thermometer (which was immersed in the liquid). The mixture was stirred and cooled with ice and salt to a temperature of from −7° to −6°. Dropwise addition was then made of 22.1 g (0.1 mole) of freshly distilled 5-benzyl-2-furoyl chloride (see Vol. 1 of this work, p. 54), b.p. 153–155°/2 mm, at such a rate that a temperature of from −4° to −3° was not exceeded (Note 1). A period of 1.5–2 hours was required for the addition of the whole of the acid chloride. When addition was complete, without removal of the bath stirring was continued until the temperature of the mixture reached that of the room (3–4 hours), and the mixture was then left overnight.
KeywordsCalcium Chloride Crude Product Heterocyclic Compound Considerable Reduction Acid Chloride
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- 1.A. L. Mndzhoian and V. G. Afrikian, Doklady Akad. Nauk Arm. SSR (Proc. Acad. Sci. Armenian SSR) 25, 201 (1957).Google Scholar