Trifluoroacetic anhydride → HCID 59562802, compound

Participants

Reaction Conditions

Reaction Steps

A 250 ml three-neck round-bottom flask which is dry and is purged with nitrogen is charged in succession with 19.7 g of the cyano alcohol (VII) (0.1 mol), 150 ml of anhydrous methylene chloride, and then 18.26 g (0.11 mol) of DBU (1,8-diazabicyclo[5.4.0]undec-7-ene). The solution is cooled to 0° C. and then 22.05 g (0.105 mol) of trifluoroacetic anhydride are added dropwise, without 5° C. being exceeded in the mass. The resulting solution is stirred at ambient temperature for 16 hours and then hydrolyzed, dried, and concentrated. The residue is distilled under vacuum (6 torr) to give 16 g of unsaturated nitrile (VIII), which distills at 105-108° C. The yield is 89%.

Provenance & Evidence