Isobutyryl chloride → HCID 59623752, compound

Participants

Reaction Steps

A mixture of 2-chloro-4-methyl-phenyl lead triacetate (0.153 g), 1-(2,2-difluoro-ethyl)-2,2-dioxo-2,3-dihydro-1H-2-λ-6-thia-1,5,8-triaza-naphthalen-4-one (Example 9.4) (0.070 g) and 4-dimethylaminopyridine (“DMAP”) (0.169 g) in anhydrous chloroform (2 ml) and toluene (1 ml) under a nitrogen atmosphere was heated to reflux for four hours. Isobutyryl chloride (53 μl) was added and the reaction mixture heated to reflux for a further two hours. The reaction mixture was then allowed to cool to ambient temperature and diluted with dichloromethane and aqueous hydrochloric acid (2M). The solids were removed by filtration and the filtrate was separated. The aqueous layer was extracted with further dichloromethane. The combined organic extracts were concentrated. The residue was purified by column chromatography on silica gel (eluent: ethyl acetate/hexane 1:6) to give Compound No. C136 of Table C (0.019 g).

Provenance & Evidence