反应详情

Oxalyl chloride (1.07 ml) was added dropwise to a stirred suspension of (R)-(+)-2-hydroxy-2-methyl-3,3,3-trifluoropropanoic acid (Method 9) (1.95 g) in dichloromethane (42 ml) and DMF (0.8 ml). The mixture was stirred at ambient temperature for 2 hours and was then added over 35 minutes to a solution of 2-chloro-4-iodoaniline (2.5 g) and 2,6-di-tert-butylpyridine (2.94 ml) in dichloromethane (40 ml) and stirred a further 18 hours. Volatile material was removed by evaporation and the residue was purified by flash chromatography on silica gel eluting with dichloromethane to give the title compound (2.85 g) as a solid. NMR: 1.6 (s, 3H), 7.7 (m, 2H), 7.8 (d, 1H), 7.9 (br s, 1H); MS: 392 (M−H)−.

1. stirringstirred a further 18 hours
2. customVolatile material was removed by evaporation
3. customthe residue was purified by flash chromatography on silica gel eluting with dichloromethane