Phosphorus oxychloride → HCID 21831324, compound

Participants

Reaction Steps

A mixture of 0.09 g of 2,2-bisfluoromethyl-3,4-dihydro-6-nitro-2H-1,3-benzoxazin-4-one, 0.18 g of phosphorus pentachloride and 1 ml of phosphorus oxychloride was stirred at room temperature for 20 minutes and the mixture was stirred at 40°-60° C. for 3 hours. The solvent was distilled off and the resultant residue was purified using silica gel column chromatography (developing solution, CH2Cl2) to obtain 0.10 g of 4-chloro-2,2-bisfluoromethyl-6-nitro-2H-1,3-benzoxazine represented by the following formula having a melting point of 75°-77° C.

Provenance & Evidence