反应详情

In 3 ml of THF was suspended 246.5 mg (1.0 mmol) of thoroughly dried cerium chloride, and 1 ml of a 1M solution of methylmagnesium bromide in THF was added thereto under an argon gas atmosphere, followed by stirring at room temperature for 1 hour. To the reaction mixture was dropwise added a solution of 245.0 mg (0.50 mmol) of Compound 63 obtained in Example 50 in 5 ml of THF, and the mixture was stirred at room temperature for 3 hours. A saturated aqueous solution of ammonium chloride was added thereto in excess to stop the reaction, followed by extraction with chloroform. The organic layer was washed and dried, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (eluent: chloroform/methanol=100/1) and recrystallized from ether to give 78.8 mg (yield: 31%) of Compound 61 as white crystals.

1. additionwas added
2. stirringthe mixture was stirred at room temperature for 3 hours
3. customthe reaction
4. extractionfollowed by extraction with chloroform
5. washThe organic layer was washed
6. customdried
7. distillationthe solvent was distilled off under reduced pressure
8. customThe residue was purified by silica gel column chromatography (eluent: chloroform/methanol=100/1)
9. customrecrystallized from ether