Water → 151539-57-0

Participants

Reaction Conditions

Reaction Steps

Compound 54 (500 mg, 1.30 mmol) obtained in Reference Example 51 was dissolved in 10 ml of dimethylformamide. To the solution were added 0.40 ml (6.43 mmol) of methyl iodide and 400 mg (6.50 mmol) of lithium carbonate, and the mixture was stirred at 80° C. for 5 hours. Water was added thereto to dissolve lithium carbonate and deposited crystals were collected by filtration. The collected crude crystals were dissolved in chloroform, washed with a saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate, followed by evaporation under reduced pressure. The residue was purified by silica gel column chromatography (eluent: chloroform), followed by recrystallization from hexane/ethyl acetate to give 162 mg (yield 31%) of Compound 64 as yellow grains.

Provenance & Evidence