Dimethylformamide → 3,3,3-Trifluoro-2,2-dimethyl-propionamide

反応式

C(Cl)(=O)C(Cl)=O.[F:7][C:8]([F:16])([F:15])[C:9]([CH3:14])([CH3:13])[C:10](O)=[O:11].C[N:18](C=O)C>C(Cl)Cl>[F:7][C:8]([F:16])([F:15])[C:9]([CH3:14])([CH3:13])[C:10]([NH2:18])=[O:11]

参加物

実験手順

Oxalyl chloride (140.8 mmol) was added dropwise to a solution of 3,3,3-trifluoro-2,2-dimethyl-propionic acid [889940-13-0] (128 mmol) in CH2Cl2 (128 mL) at 0° C. Added a few dr DMF until gas evolution was observed and then continued stirring for 30 min. After warming to rt and stirring overnight, the reaction mixture was concentrated (40° C., 00 mbar). The residue was dissolved in THF (128 mL), cooled to 0° C. and then slowly treated with a solution of concentrated aqueous ammonia (64 mL). After stirring at 0° C. for 30 min and then at rt for 4 h, the reaction mixture was concentrated to half its volume to give a thick white suspension. After filtering and drying, the title compound was obtained as a white solid. ESI-MS: [M+H]+ 156.