反应详情

温度

60 °C

6Methyl-pyrido[3,4-d]pyrimid-4one (200 mg, 1.24 mmol), polymer-supported triphenylphosphine (2.06 g of 3.0 mmol Pig resin, 6.20 mmol) and anhydrous carbon tetrachloride (1.20 mL, 12.40 mmol) were combined in 1,2-dichloroethane (6 mL). The mixture was heated to 60° C. under an atmosphere of dry N2(g) for 18 hours. 6-Chloroindoline (1.1 eq.) was added and heating was continued at 60° C. for another 18 hours. The triphenyphosphine-bearing resin was filtered off and washed several times with chloroform. The filtrate and washings were concentrated in vacuo and preparative reversed-phase (C18) chromatography utilizing a gradient of 15% to 70% MeCN/pH4.5, 50 mM NH4OAc followed by lyophilization of the appropriate fractions afforded the title product (30%) as its free-base: MP: 232-234° C.; LC-MS: 297 (MH+); anal. RP-HPLC: 4.33 minutes.

1. temperatureheating
2. filtrationThe triphenyphosphine-bearing resin was filtered off
3. washwashed several times with chloroform
4. concentrationThe filtrate and washings were concentrated in vacuo