Trifluoroacetic acid methylene chloride → HCID 66726889, compound

Participants

Reaction Steps

A product of Example 2, Step C (1.32 g; 2.71 mmol) in 60% CF3CO2H/CH2Cl2 (10 ml) was stirred for 10 min at room temperature under N2, then diluted to 30 ml with EtOH and stirred for additional 15 min. This was evaporated to dryness under reduced pressure and the residue was dissolved in EtOAc (10 ml) and hexane (20 ml) was added. After standing overnight at room temperature, the precipitate formed was filtered off, washed with hexane and dried to give the title compound (0.77 g; 79%), as off white solid, which was used in the next step without further purification. 1H-NMR (CDCl3) 4.47 (5, 2H); 4.51 (s, 2H); 6.7-6.8 (m, 1H); 7.0-7.21 (m, 1H); 7.4-7.7 (m, 1H); 10.6 (broad s, 1H).

Provenance & Evidence