HCID 58387154, compound → HCID 58387188, compound

Participants

Reaction Conditions

Reaction Steps

A 5 mL Biotage™ microwave vial was charged with Fe (285.0 mg, 5.11 mmol), a solution of compound 2-1 (166.0 mg, 0.511 mmol) in EtOH (3 mL) and diluted aqueous HCl (82 uL of 37% aqueous HCl, diluted with 0.75 mL of water). The resulting suspension was heated in a microwave synthesizer (Biotage Initiator™) at 130° C. for 10 min. The mixture was then filtered and the remaining solids were washed with EtOAc (three times, 2 mL). The filtrate and washes were combined and evaporated to dryness in vacuo. The residue was dissolved in 3:1 EtOAc/TEA and passed through a short plug of a neutral alumina. The resulting solution was evaporated to dryness in vacuo to give the crude product as brownish oil. LR-MS (API-ES): calculated for C18H15ClN2 294.1, observed m/e 295.0 (M+H)+ (Rt 3.07 min). The crude product was used in the next step without further purification.

Provenance & Evidence