Sodium Bisulfate → HCID 13509661, compound

Temperature

-20 °C

Lithium aluminum hydride (0.5 g, 11.7 mmol) was suspended in ether (50 ml) and cooled to −20° C. to −30° C. Thereto was added dropwise a solution of ethyl 2,2-dimethyl-3-hydroxy(2-chlorobenzoyl)acetate (2 g, 7.8 mmol) in ether (10 ml) while maintaining at not higher than −20° C. The mixture was stirred at −20° C. for 1 h and at 0° C. for 3 h, cooled to −20° C. and 10%—NaHSO4 aqueous solution (20 ml) was added dropwise. The mixture was stirred at room temperature for 30 min, and an insoluble material was removed by decantation. This was washed twice with ether (100 ml) and the organic layer was combined. The mixture was washed with water, dried over anhydrous sodium sulfate, and concentrated to dryness to give the title compound (1.3 g, 78%) as a colorless oil.

1. temperaturecooled to −20° C. to −30° C
2. temperaturecooled to −20° C.
3. stirringThe mixture was stirred at room temperature for 30 min
4. customan insoluble material was removed by decantation
5. washThis was washed twice with ether (100 ml)
6. washThe mixture was washed with water
7. dry with materialdried over anhydrous sodium sulfate
8. concentrationconcentrated to dryness

ORD record

ord-6b1acb824f1c46b7bf6dd447ccf2be28

Source dataset

uspto-grants-2004_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06800778B1