反应详情

温度

100 °C

To a mixture of 4-(4-amino-phenyl)-piperazine-1-carboxylic acid tert-butyl ester (133 mg, 0.48 mmol) and sodium tert-butoxide (57.6 mg, 0.6 mmol) in 1,4-dioxane (0.5 mL) is added a solution of 2-chloro-7-(1-ethyl-propyl)-7H-pyrrolo[2,3-d]pyrimidine (90 mg, 0.4 mmol) in 1,4-dioxane (1.0 mL), Pd2(dba)3 (18.3 mg, 0.02 mmol) and BINAP (25 mg, 0.04 mmol). The mixture is degassed, and heated at 100° C. for 3 h. The mixture is cooled to room temperature, diluted with EtOAc, and filtered through celite. The filtrate is concentrated under reduced pressure. The residue is purified by flash chromatography (SiO2, EtOAc:Hexane=1:1) to give 167 mg of 4-{4-[7-(1-ethyl-propyl)-7H-pyrrolo[2,3-d]pyrimidin-2-ylamino]-phenyl}-piperazine-1-carboxylic acid tert-butyl ester as a pale yellow solid.

1. customThe mixture is degassed
2. temperatureThe mixture is cooled to room temperature
3. additiondiluted with EtOAc
4. filtrationfiltered through celite
5. concentrationThe filtrate is concentrated under reduced pressure
6. customThe residue is purified by flash chromatography (SiO2, EtOAc:Hexane=1:1)