反应详情

To a solution of the compound of Example 1-2 (68 mg, 0.11 mmol) in N,N-dimethylformamide (1.1 mL) were added zinc cyanide (15 mg, 0.13 mmol) and tetrakistriphenylphosphine palladium (25 mg, 0.02 mmol), and the reaction was carried out at 80° C. for 2 hours. To the reaction solution was added saturated aqueous sodium bicarbonate, and the mixture was extracted with toluene-ethyl acetate (1:1). The organic layer was dried over magnesium sulfate and filtered, and then evaporated and purified by silica gel column chromatography (chloroform/methanol/ammonia water=50/1/0 to 10/1/0 to 100/10/1) to give the titled compound (54 mg, 94%).

1. extractionthe mixture was extracted with toluene-ethyl acetate (1:1)
2. dry with materialThe organic layer was dried over magnesium sulfate
3. filtrationfiltered
4. customevaporated
5. custompurified by silica gel column chromatography (chloroform/methanol/ammonia water=50/1/0 to 10/1/0 to 100/10/1)