Formic Acid → HCID 84071213, compound

Temperature

200 °C

A solution (1 mL) of the compound (560 mg, 2.28 mmol) of Step 1 in N-methyl-2-pyrrolidinone was irradiated with a microwave in a tightly-sealed container, and stirred at 200° C. for 1 hour. To the reaction solution, ethyl acetate and hexane were added. After washing with water and saturated brine, the resultant was dried over anhydrous magnesium sulfate. The solvent was distilled away under reduced pressure. The residue was purified by silica gel chromatography. To the resulting compound (368 mg, 1.50 mmol), formic acid (2 mL) and water (0.2 mL) were added, and stirred at 100° C. overnight. The reaction solution was diluted with ethyl acetate, and after washed with water and saturated brine, the resultant was dried over anhydrous magnesium sulfate. The solvent was distilled away under reduced pressure. The resulting residue was purified by silica gel chromatography (hexane/ethyl acetate) to thus obtain the title compound.

1. washAfter washing with water and saturated brine
2. dry with materialthe resultant was dried over anhydrous magnesium sulfate
3. distillationThe solvent was distilled away under reduced pressure
4. customThe residue was purified by silica gel chromatography
5. stirringstirred at 100° C. overnight
6. washafter washed with water and saturated brine
7. dry with materialthe resultant was dried over anhydrous magnesium sulfate
8. distillationThe solvent was distilled away under reduced pressure
9. customThe resulting residue was purified by silica gel chromatography (hexane/ethyl acetate)

ORD record

ord-2a06de5216474f36bcc9cd889862244d

Source dataset

uspto-grants-2016_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09290487B2