2,2,2-Trifluoroethanol → HCID 59726030, compound

Participants

Reaction Steps

A solution of 2,2,2-trifluoroethanol (329 mg, 3.28 mmol) in 3.0 mL of THF and 3.0 mL of DMF at 0° C. was treated with sodium hydride (60% wt) (131 mg, 3.28 mmol) and the resulting mixture was stirred for 10 min, then solid 6-bromo-1-chlorophthalazine (400 mg, 1.64 mmol) was added in one portion. The mixture was stirred at RT for 1 h, poured into iced-cold saturated NH4Cl solution, and extracted with EtOAc twice. The combined organic layers were dried over sodium sulfate, concentrated under vacuum. The residue was put on an ISCO 40 g column (eluted with 20-70% EtOAc in Hexanes) and purified to give title compound as a tan amorphous solid. MS (ESI, pos. ion) m/z: 309.0 (M+1).

Provenance & Evidence