Ethanol → HCID 86728491, compound

Participants

Reaction Conditions

Reaction Steps

Under a nitrogen atmosphere, the oily product of step 3 (15.0 g) was dissolved in 2,2,2-trifluoroethanol (33 mL) Resorcinol (5.3 g, 47.9 mmol) and methanesulfonic acid (11.7 mL, 181 mmol) were added thereto at 24° C., and the mixture was stirred at 90° C. for 4 hours. The mixture was cooled to room temperature and allowed to stand for 13 hours, ethanol (33 mL) and water (11 mL) were then added, and the mixture was stirred at 90° C. for 4.5 hours. It was cooled to 55° C., 2-propanol (105 mL) was added, and the mixture was cooled to room temperature and allowed to stand for 14 hours. The precipitated crystals were collected by filtration, washed twice with 2-propanol (33 mL), and dried under reduced pressure to obtain the title compound (8.2 g).

Provenance & Evidence