Triethylamine → HCID 69222621, compound

Participants

Reaction Conditions

Reaction Steps

In a pressure tube, 200 mg (0.64 mmol) of 3-[5-(6-chloro-pyridin-3-yl)-isoxazol-3-yl]-benzoic acid, 97 mg (0.96 mmol, 1.5 eq.) of triethyl amine and 166 mg (1.9 mmol, 3.0 eq.) of isobutyl-methyl-amine are dissolved in 3 ml of THF. The reaction mixture is heated to 120° C. and after 6 h to 150° C. After 60 h, the mixture is cooled to room temperature and the solvent is removed. After addition of 10 ml of water, the pH is adjusted to 2 and the precipitate filtered off. The solid is then dissolved in 10 ml of methanol and 5 ml of dichloroethane, precipitated through addition of 10 ml of hexane and filtered. Recrystallisation from 15 ml of dichloromethane and 1 ml of methanol yields the title compound as a white solid. Mass spectrum: m/z (M+H)+: 352.2

Provenance & Evidence