Hydrazine hydrate (1:1) → HCID 178507266, compound

Temperature

75 °C

To a solution of 126a (477 mg, 4.38 mmol) in methanol (5 mL) was added hydrazine hydrate (5 mL, 80%). The reaction mixture was heated at 75° C. for 15 h. The methanol was removed under reduced pressure and the residue was extracted with dichloromethane (2×8 mL). The combined extract was dried over Na2SO4 and concentrated. The residue was purified by flash column eluting with 100:1 dichloromethane/methanol to afford 126b as a yellow oil (250 mg, 46%, over two steps). MS: [M+H]+ 124.

1. customThe methanol was removed under reduced pressure
2. extractionthe residue was extracted with dichloromethane (2×8 mL)
3. extractionThe combined extract
4. dry with materialwas dried over Na2SO4
5. concentrationconcentrated
6. customThe residue was purified by flash column
7. washeluting with 100:1 dichloromethane/methanol

ORD record

ord-88610df068c5463ebeb89141e5da1e97

Source dataset

uspto-grants-2014_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08754077B2