Triethylamine → HCID 86704615, compound

Participants

Reaction Steps

A mixture of the title compound from Step A (20 mg, 0.030 mmol) and mCPBA (10.50 mg, 0.061 mmol) in CH2Cl2 (2 mL) was stirred at room temperature for 1 h. TLC showed no SM. The mixture was diluted with CH2Cl2 (10 mL) and washed with Na2S2O3 and Na2HCO3, and dried over Na2SO4. The solvent was removed. A mixture of the residue, 3,3-difluoro-azetidine (19.70 mg, 0.152 mmol) and Et3N (3.08 mg, 0.030 mmol) in THF was heated at 140° C. under microwave for 4 h. The solvent was removed and the title compound was purified by preparative TLC plate as a white solid using EtOAc/hexane as the elute (2/8). LCMS=703.4 (M+H)+. The final compound was a mixture of two separable atropisomers, which could be separated by chiral OD column using EtOH/heptane as the elute.

Provenance & Evidence