反应详情

温度

100 °C

Compound 71 was prepared according to general method H. A 15 mL Schlenk tube was charged with (R)-(4-(4-chlorophthalazin-1-yl)-3-methylpiperazin-1-yl)(cyclohexyl)methanone JK-5 (130 mg, 349 μmol), 4-carbamoylphenylboronic acid (77 mg, 523 μmol), tris(dibenzylideneacetone)dipalladium (0) (3.2 mg, 3.5 μmol), dicyclohexyl(2,6-dimethoxyphenyl)phosphine (2.3 mg, 7.0 μmol), and potassium phosphate tribasic (148 mg, 697 μmol). The vessel was evacuated, backfilled with argon 5 times, and then previously degassed n-butanol (1 mL) was added. The reaction was heated at 100° C. for 20 hours. After cooling, the reaction was added to aqueous K2CO3 (10%) and extracted three times with dichloromethane. The combined organics were dried (MgSO4) and evaporated to give a yellow oil. Chromatography over silica gel with a gradient of hexanes/0-100% ethyl acetate gave a pale yellow solid, compound 71. MS (M+H)+=452.2.

1. customCompound 71 was prepared
2. customThe vessel was evacuated
3. additionpreviously degassed n-butanol (1 mL) was added
4. temperatureAfter cooling
5. additionthe reaction was added to aqueous K2CO3 (10%)
6. extractionextracted three times with dichloromethane
7. dry with materialThe combined organics were dried (MgSO4)
8. customevaporated
9. customto give a yellow oil