2-Bromopropane → 3-[4-(Benzyloxy)phenyl]-6-fluoro-1-(1-methylethyl)-1H-pyrazolo[4,3-b]pyridine

温度

90 °C

A mixture of [4-(benzyloxy)phenyl](3,5-difluoropyridin-2-yl)methanone (100 mg) and hydrazine hydrate (77 mg) in 2-propanol (5 mL) was stirred at room temperature for 30 min and at 90° C. for 12 h, treated with water, and extracted with AcOEt. The organic layer was dried over MgSO4 and concentrated under reduced pressure. The residue was dissolved in DMF (5 mL), and then Cs2CO3 (150 mg, 0.46 mmol) and 2-bromopropane (50.5 mg) were added successively. The mixture was stirred for 12 h, treated with water, and extracted with AcOEt. The organic layer was dried over MgSO4 and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (AcOEt/hexane) to give the title compound (70.0 mg).

1. extractionextracted with AcOEt
2. dry with materialThe organic layer was dried over MgSO4
3. concentrationconcentrated under reduced pressure
4. dissolutionThe residue was dissolved in DMF (5 mL)
5. stirringThe mixture was stirred for 12 h
6. extractionextracted with AcOEt
7. dry with materialThe organic layer was dried over MgSO4
8. concentrationconcentrated under reduced pressure
9. customThe residue was purified by silica gel column chromatography (AcOEt/hexane)

ORDレコード

ord-06fe055b39794ab5aaf1dbe4da08b2ec

出典データセット

uspto-grants-2015_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09029536B2