HCID 117689908, compound → HCID 90384192, compound

Temperature

140 °C

A polyphosphoric acid (1.86 g) was suspended in chlorobenzene (8 mL), and a solution (8 mL) of the compound (730 mg, 2.60 mmol) of Step 1 of Example 51 in chlorobenzene was added thereto at 120° C., and stirred at 140° C. overnight. After further stirred at 155° C. two nights, the resultant was returned to room temperature, and the reaction solution was concentrated under reduced pressure, and diluted with ethyl acetate. To the mixture liquid, a 1 N sodium hydroxide aqueous solution was added under ice-cooling for the neutralization, and the insoluble material was filtered off. The filtrate was extracted with ethyl acetate, washed with saturated brine, and then dried over anhydrous magnesium sulfate. The resultant was concentrated under reduced pressure. The resulting residue was purified by silica gel chromatography (hexane) to thus obtain the title compound.

1. stirringAfter further stirred at 155° C. two nights
2. customwas returned to room temperature
3. concentrationthe reaction solution was concentrated under reduced pressure
4. additiondiluted with ethyl acetate
5. additionTo the mixture liquid, a 1 N sodium hydroxide aqueous solution was added under ice-
6. temperaturecooling for the neutralization
7. filtrationthe insoluble material was filtered off
8. extractionThe filtrate was extracted with ethyl acetate
9. washwashed with saturated brine
10. dry with materialdried over anhydrous magnesium sulfate
11. concentrationThe resultant was concentrated under reduced pressure
12. customThe resulting residue was purified by silica gel chromatography (hexane)

ORD record

ord-6b48b7df4bf74eb9ad41de219adb6530

Source dataset

uspto-grants-2016_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09290487B2