反应详情

温度

140 °C

(Tert-butyldimethylsilyloxymethyl)tri-n-butyltin (Tetrahedron Vol. 45, No. 4, 993-1006: 121 mg) and tetrakistriphenylphosphinepalladium (13.4 mg) were added to a N-methylpyrrolidone (2.5 ml) solution of the compound 323-4 (100 mg), and the obtained mixture was stirred at 140° C. for 6 hours. The temperature of the reaction solution was returned to room temperature. Thereafter, THF (2 ml) and tetrabutyl ammonium fluoride (1 M THF solution: 232 ul) were added to the reaction solution, and the obtained mixture was stirred at room temperature for 14 hours. Water was added to the reaction solution, and the mixture was extracted with ethyl acetate. The obtained organic layer was washed with a saturated sodium chloride aqueous solution, dried over magnesium sulfate, and then concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (n-heptane:ethyl acetate=19:1 to 1:1), so as to obtain the title compound (26.6 mg).

1. customwas returned to room temperature
2. stirringthe obtained mixture was stirred at room temperature for 14 hours
3. extractionthe mixture was extracted with ethyl acetate
4. washThe obtained organic layer was washed with a saturated sodium chloride aqueous solution
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. customThe obtained residue was purified by silica gel column chromatography (n-heptane:ethyl acetate=19:1 to 1:1)