Pyridine → HCID 71471186, compound

Participants

Reaction Steps

2-chloroisonicotinic acid 8.1.A (5000 mg, 31735 μmol) was refluxed in SOCl2 overnight under nitrogen. Another 4 mL of SOCl2 was added in the morning. After 2 hr., solution cleared up. The r×n was then concentrated and added to a thiosemicarbazide (2892 mg, 31735 μmol)/pyridine solution at 0° C. After 4 hr., LC/MS showed product MS along with many side peaks. The reaction was stopped and concentrated. Water and a small amount of EtOAc were added, precipitates were generated. Filtered and washed the precipitates with water 4 times. The solids were dried. LC/MS and the NMR of the precipitates showed to be the pure product. 4.05 g of the product 8.1.B (55%) was generated as a yellow powder.

Provenance & Evidence