Dichloromethane → HCID 11618343, compound

Participants

Reaction Steps

To an oven dried 10 mL round bottom flask was added 5 mL of DCM, 20 mg (0.04 mmol) of 331, 1.5 mL trifluoroacetic acid (TFA), and 50 μL H2O. The reaction solution was stirred for 1 hour and quenched with 1 mL of saturated NaHCO3. The product was taken up in 20 mL of DCM and the organic solution further washed with water (3×15 mL) and dried over Na2SO4. The organic solution was rotary evaporated to provide 16.0 mg of the product as a pale tan oil (99.0% yield). 1H NMR 400 MHz DMSO-d6: δH 8.71 (1H, dd, J=2.7, 3.1 Hz), 8.48 (1H, br s), 8.07 (1H, br s), 7.90 (1H, s), 7.83-7.30 (10H, m); 3.28-1.16 (11H, m); MS (ES+) m/z 405 (M+H); HPLC (214 nm), rt 4.94 min, 99.8%.

Provenance & Evidence