反应详情

A mixture of 41.1 g (274 mmol) 4-carboxybenzaldehyde, 50 g (274 mmol) 1,1,1,3,3,3-hexafluoro-2-methyl-2-propanol, and 33.4 g (274 mmol) DMAP in 700 mL DCM was stirred until homogeneous (approximately 0.5 hr). The solution was cooled over an ice bath, under Ar, and 52.3 g (274 mmol) EDCI was added portion-wise. The reaction was stirred at RT for 48 hr. and concentrated to an oil on the rotovap. The oil was taken up with EA and washed with water, 2× with dil. Citric acid, 2× with dil. Sodium bicarbonate, and brine. The organic layer was dried over sodium sulfate and concentrated to 25.5 g pale yellow solid.

1. additionwas added portion-wise
2. stirringThe reaction was stirred at RT for 48 hr
3. concentrationand concentrated to an oil on the rotovap
4. washwashed with water, 2× with dil. Citric acid, 2× with dil. Sodium bicarbonate, and brine
5. dry with materialThe organic layer was dried over sodium sulfate
6. concentrationconcentrated to 25.5 g pale yellow solid