Ethyl chloroformate → HCID 14171567, compound

Participants

Reaction Steps

To a stirred slurry of 1-amino-2-(2,4-dichlorobenzoyl)pyrrole (377.6 g) and sodium bicarbonate (286.0 g) in 2.0 L of dichloromethane was added ethyl chloroformate (176.90 g) over 10 min. The reaction mixture was heated at reflux for 4 hrs and then quenched with H2O. The organic layer was washed with brine, dried (MgSO4), charcoaled, filtered and concentrated to a maroon oil. This oil was purified by flash chromatography (silica, dichloromethane) and concentrated to a green powder which was recrystallized from ether to give 171.8 g of white crystals, mp 114°-116°.

Provenance & Evidence