反应详情

温度

110 °C

Dissolve 1,3-dimethyl-1H-pyrazole-4-sulfonic acid [2-(3′-chloro-2,3,5,6-tetrahydro-[1,2′]bipyrazinyl-4-yl)-ethyl]-methyl-amide (270 mg, 0.652 mmol) in DMA-H2O (10 ml; 3:1 v/v, previously degassed with nitrogen). Add 4-methoxymethylphenyl boronic acid (130 mg, 0.783 mmol), potassium carbonate (216 mg, 1.56 mmol) and tetrakis(triphenylphosphine)palladium (38 mg, 0.0326 mmol). Heat the reaction mixture at 110° C. for 18 hr. Cool and dilute with ethyl acetate and water. Extract the aqueous layer with ethyl acetate and combine the organic layers. Wash the organic layers with brine and concentrate. Purify by chromatography, eluting with 1:2 hexanes:acetone to afford the free base of the title compound (182 mg, 56% yield) as a white foam.

1. custom3:1 v/v, previously degassed with nitrogen)
2. temperatureCool
3. extractionExtract the aqueous layer with ethyl acetate
4. washWash the organic layers with brine
5. concentrationconcentrate
6. customPurify by chromatography
7. washeluting with 1:2 hexanes