1,2-Dichloroethane → HCID 53740309, compound

Participants

Reaction Steps

2.4 g (16.1 mmol) 3-(3-pyridyl)-acrylic acid and 5.3 ml (38.0 mmol) TEA are suspended in 80 ml abs. dichloromethane and cooled to ca. 0° C. under moisture exclusion. 2.9 g (18.9 mmol) 88% HOBT and 3.6 g (18.8 mmol) EDC are added and the mixture is stirred for 30 min under ice cooling. 5.3 g (17.0 mmol) 4-(trans-2-phenyl-cyclopropyl-carbonylamino)-butylamine are dissolved in 30 ml abs. dichloromethane and added drop-wise under ice cooling. The mixture is stirred overnight at RT without further cooling. The formed precipitate is filtered off and crystallized from 120 ml isopropanol. Colorless crystals with MP. 194-196° C. Yield 4.2 g (71%).

Provenance & Evidence