Methanol → HCID 16765315, compound

Temperature

80 °C

To a suspension of ethyl (5-oxo-2,5-dihydro-1H-pyrazol-3-yl)acetate obtained in Reference Example 117 (5.00 g, 29.4 mmol) in THF (20 mL)-methanol (20 mL)-water (20 mL) was added 5N aqueous sodium hydroxide solution (11.0 mL, 88.0 mmol) at room temperature, and the mixture was stirred under heating at 80° C. for 3 hr. The reaction mixture allowed to cool to room temperature, and concentrated under reduced pressure, and the residue was diluted with water, and acidified with 6N hydrochloric acid. The precipitated solid was collected by filtration, and washed with water, and dried under nitrogen stream to give the title compound as a white powder (3.43 g, 82%).

1. temperatureto cool to room temperature
2. concentrationconcentrated under reduced pressure
3. additionthe residue was diluted with water
4. filtrationThe precipitated solid was collected by filtration
5. washwashed with water
6. customdried under nitrogen stream

ORD record

ord-6de0b517e36f403b8d8c09f3adb76c16

Source dataset

uspto-grants-2011_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07915267B2