Triethylamine → HCID 67494121, compound

Participants

Reaction Steps

To a suspension of the product of step 3 (0.3 g) in anhydrous dichloromethane (30 ml), a solution of 4-fluoroaniline (0.1 g) and triethylamine (0.2 ml) in dichloromethane (15 ml) was added dropwise slowly in an ice-bath with the temperature no more than 5° C. After addition, the reaction was carried out for 30 min in an ice-bath, and then at room temperature overnight. The completion of reaction was indicated by TLC. Potassium carbonate solution (10%) was added. The reaction mixture was extracted with EtOAc (20 ml*3). The organic layer was dried over anhydrous MgSO4, filtered, and concentrated under reduced pressure to recover solvent. The residue was purified on a silica gel column using EtOAc/petroleum ether/ethanol (1:2:0.5) as an eluent. The concentration of the eluent and crystallization provided a solid powder.

Provenance & Evidence