反应详情

温度

105 °C

A 44-mL sealed tube equipped with a magnetic stirrer was charged with 220a (400 mg, 1.0 mmol), 7 (508 mg, 2.0 mmol), potassium acetate (392 mg, 4.0 mmol) and 1,4-dioxane (10 mL). After the mixture was degassed for 30 minutes, Pd(dppf)Cl2.CH2Cl2 (82 mg, 0.10 mmol) was added. The resulting reaction mixture was stirred at 105° C. for 6 h. Then, it was cooled to room temperature and filtered through a pad of Celite. The filtrate was concentrated, and the crude mixture was redissolved in DME (2 mL) and transferred into a 10-mL microwave reaction vessel. To this solution was added 10-[2-(acetoxymethyl)-3-bromo-5-fluorophenyl]-4,4-dimethyl-1,10-diazatricyclo-[6.4.0.02,6]dodeca-2(6),7-dien-9-one (189a) (270 mg, 0.60 mmol), Pd(PPh3)4 (50 mg, 0.050 mmol), and 2 N Na2CO3 (2 mL). Then, the reaction mixture was degassed for 5 minutes and placed into the microwave cavity. After the reaction mixture was stirred at 125° C. for 7 min., it was purified by flash chromatography (dichloromethane:methanol, 85:15) to give 49% (150 mg) of 245a.

1. customA 44-mL sealed tube
2. customequipped with a magnetic stirrer
3. customAfter the mixture was degassed for 30 minutes
4. customThe resulting reaction mixture
5. temperatureThen, it was cooled to room temperature
6. filtrationfiltered through a pad of Celite
7. concentrationThe filtrate was concentrated
8. dissolutionthe crude mixture was redissolved in DME (2 mL)
9. customtransferred into a 10-mL microwave reaction vessel
10. customThen, the reaction mixture was degassed for 5 minutes
11. stirringAfter the reaction mixture was stirred at 125° C. for 7 min.
12. customit was purified by flash chromatography (dichloromethane:methanol, 85:15)