Trifluoroacetic acid → HCID 21638785, compound

Participants

Reaction Steps

The product from Step A (11 g) was suspended in CH2Cl2 (75 mL), and TFA was added dropwise (75 mL). The resulting solution was stirred overnight at ambient temperature. The reaction solution was concentrated under reduced pressure, and the resulting residue was dissolved in CH2Cl2 (100 mL). Saturated aqueous NaHCO3 (100 mL) was added slowly with stirring. After 20 min the organic layer was separated, washed with water (10 mL) and then brine (30 mL), and dried over Na2SO4. The organic layer was then concentrated under reduced pressure and purified via silica gel chromatography (0-35% methanol/dichloromethane) to give the title compound (7.6 g). MS (electrospray): exact mass calculated for C13H14ClN3O, 263.08; m/z found, 264.1 [M+H]+.

Provenance & Evidence