1,2-Dichloroethane → HCID 20190402, compound

Participants

Reaction Conditions

Reaction Steps

A solution of 3-(3-pyridyl)-5,6,7,8-tetrahydroindolizine-1-carboxylic acid (13.3 g) in a mixture of thionyl chloride (19.2 cc), dimethylformamide (0.05 cc) and 1,2-dichloroethane (160 cc) is heated to a temperature of about 70° C. The suspension obtained is kept at a temperature of about 70° C. for 3 hours. The reaction mixture is cooled to a temperature of about 20° C. and concentrated to dryness under reduced pressure (20 mm Hg; 2.7 kPa) at a temperature of about 60° C. The residue is suspended in cyclohexane (300 cc) and the solvent is evaporated off under reduced pressure (20 mm Hg; 2.7 kPa) at a temperature of about 60° C. The same operation is repeated twice. 1-Chloroformyl-3-(3-pyridyl)-5,6,7,8-tetrahydroindolizine hydrochloride (16.3 g) is thus obtained in the form of light green crystals melting at 205° C.

Provenance & Evidence