1,2-Dichloroethane → HCID 21084087, compound

Participants

Reaction Steps

EDC (66 mg, 0.35 mmol) and HOBT (43 mg, 0.32 mmol) were added to the compound of Example 59 (100 mg, 0.29 mmol) in DCM (2 mL). After 15 min ethylamine hydrochloride (26 mg, 0.32 mmol) and NMM (0.070 mL, 0.63 mmol) were added and the reaction mixture was stirred at r.t. overnight. Water (2 mL) and DCM (2 mL) were added, the suspension filtered through a hydrophobic frit and the organic phase concentrated in vacuo. The crude product was purified by column chromatography on silica (1% MeOH in DCM) to give the title compound as a white solid (95 mg, 88%). δH (DMSO-d6) 7.69–7.61 (3H, m), 7.59–7.49 (3H, m), 7.45 (1H, d, J 9.6 Hz), 7.44–7.42 (4H, m), 7.05 (1H, t, J 5.4 Hz), 6.54 (1H, d, J 9.6 Hz), 3.03 (2H, q, J 7.1 Hz), 0.84 (3H, t, J 7.1 Hz). LCMS (ES+) RT 3.33 minutes, 375.0 (M+H)+.

Provenance & Evidence