Acetone → HCID 23298004, compound

Participants

Reaction Conditions

Reaction Steps

355 ml of a 15% titanium trichloride solution in aqueous hydrochloric acid are dissolved in 850 ml of water and 850 ml of acetone under a nitrogen atmosphere at 0° C. A solution of 35.5 g (110.8 mmol) of ethyl N-(2-methyl-6-nitro-4-trifluoromethylphenyl)oxamate in 1.7 1 of acetone is slowly added dropwise. The resulting violet solution is stirred at 0° C. for 16 hours. 15% titanium trichloride solution in aqueous hydrochloric acid is then added until, according to 1H-NMR analysis, starting material is no longer detectable. The reaction mixture is filtered off on a suction filter, the filtrate is concentrated and the deposited solid is filtered off again on a suction filter. The crude product is washed with dilute hydrochloric acid and water. The title compound is obtained as a white solid.

Provenance & Evidence