Potassium Carbonate → N-tert-butyl-2-(5-(difluoromethoxy)-1-(4-methyl-4-nitropentyl)-1H-indazol-3-yl)-5-trityl-5H-pyrrolo[3,2-b]pyrazine-7-carboxamide

温度

100 °C

To a solution of N-tert-butyl-2-(5-(difluoromethoxy)-1H-indazol-3-yl)-5-trityl-5H-pyrrolo[3,2-b]pyrazine-7-carboxamide (208 mg, 0.35 mmol) in DMF (15 mL) was added K2CO3 (193 mg, 1.4 mmol) and 1-chloro-4-methyl-4-nitropentane (100 mg, 0.59 mmol), after the addition, the reaction mixture was heated to 100° C. with stirring for 4 hours. Then, the mixture was quenched with H2O (25 mL) and product extracted with EtOAc (50 mL). The organic layer was washed with H2O (100 mL), brine (100 mL), dried over Na2SO4 and concentrated under reduced pressure to give N-tert-butyl-2-(5-(difluoromethoxy)-1-(4-methyl-4-nitropentyl)-1H-indazol-3-yl)-5-trityl-5H-pyrrolo[3,2-b]pyrazine-7-carboxamide (200 mg, 69%) as yellow solid, material used in the next step without further purification. LCMS: (M+H)+=772; (M+Na)+=794.0.

1. additionafter the addition
2. customThen, the mixture was quenched with H2O (25 mL) and product
3. extractionextracted with EtOAc (50 mL)
4. washThe organic layer was washed with H2O (100 mL), brine (100 mL)
5. dry with materialdried over Na2SO4
6. concentrationconcentrated under reduced pressure

ORDレコード

ord-2e4f3a71d1b14b5fb21d3d4492c64337

出典データセット

uspto-grants-2014_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08658646B2