反应详情

温度

195 °C

To a solution of 1,4-dichloro-6,7-dihydro-5H-cyclopenta[d]pyridazine (150 mg, 0.79 mmol) in NMP (5 mL) is added (S)-3-methyl-3,4,5,6-tetrahydro-2H-[1,2′]bipyrazinyl-5′-carboxylic acid ethyl ester (297 mg, 1.19 mmol) and triethyl amine (332 μL, 2.39 mmol). The reaction mixture is heated in a microwave reactor at 195° C. for 4 h. Water and EtOAc is added. The layers are separated and the aqueous layer is extracted with EtOAc. The combined organic layers are washed with water, brine, dried over Na2SO4, filtered and concentrated. The crude product is purified by flash chromatography (EtOAx/heptane 10% to 70%) to yield 50 mg (16%) of the title compound.

1. customThe layers are separated
2. extractionthe aqueous layer is extracted with EtOAc
3. washThe combined organic layers are washed with water, brine
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe crude product is purified by flash chromatography (EtOAx/heptane 10% to 70%)