反应详情

温度

100 °C

A degassed mixture of (4-{7-[bis-(2-trimethylsilanyl-ethoxymethyl)-amino]-6-bromo-3-quinolin-3-yl-pyrazolo[1,5-a]pyrimidin-5-yl}-cyclohexyl)-acetic acid ethyl ester (0.078 mmol, 60 mg), Bu3SnCN (50 mg, 0.156 mmoL), Pd[P(t-Bu)3]2 (8.3 mg, 0.016 mmoL) in Dioxane (1 mL) was heated at 100° C. for 18 h. The reaction mixture was concentrated in vacuo. The crude mixture was dissolved in 2:1 MeOH:H2O (1.5 mL) and was treated with 2N NaOH(aq) (0.5 mL). The resulting reaction mixture was stirred at room temperature for 18 hours. Aqueous hydrochloride solution (1.0 N, 2 ml) was added to the reaction mixture and the resulting solution was stirred at 65° C. for 2 h. The solution was concentrated and purified by prep-LC to afford the title compound (8.8 mg) as a mixture of cis and trans isomers: LC/MS RT=3.88 min. Mass calculated for, M+H 427.18, observed 427.18.

1. concentrationThe reaction mixture was concentrated in vacuo
2. dissolutionThe crude mixture was dissolved in 2:1 MeOH
3. additionH2O (1.5 mL) and was treated with 2N NaOH(aq) (0.5 mL)
4. customThe resulting reaction mixture
5. stirringthe resulting solution was stirred at 65° C. for 2 h
6. concentrationThe solution was concentrated
7. custompurified by prep-LC