Potassium Sodium Tartrate → HCID 131725171, compound

Temperature

-50 °C

5.7 g of the above product (a) was dissolved in 150 ml of toluene, and the solution was cooled to −50° C. To the solution was added 20 ml of a solution (1.0M) of diisobutyl alminum lithium hydride (DIBAL) in toluene. The solution was stirred at −50° C. for one hour. To the reaction solution was added 26 ml of DIBAL solution, followed by stirring for further twenty minutes. Then, to the reaction solution was added 50 ml of a saturated ammonium chloride solution, followed by stirring at room temperature for ten minutes. To the reaction solution was added 10 g of Rochelle salt, followed by stirring for further thirty minutes and filtering through Celite. The filtrate was washed with a saturated Rochelle salt solution and a saturated saline solution, and dried over anhydrous sodium sulfate, and the solvent was evaporated. The residue was purified by column chromatography on silica gel, and the eluate with ethyl acetate-hexane (1:8) was collected, to afford 3.9 g of the titled compound (b) as a colorless oily matter.

1. stirringby stirring for further twenty minutes
2. stirringby stirring at room temperature for ten minutes
3. stirringby stirring for further thirty minutes
4. filtrationfiltering through Celite
5. washThe filtrate was washed with a saturated Rochelle salt solution
6. dry with materiala saturated saline solution, and dried over anhydrous sodium sulfate
7. customthe solvent was evaporated
8. customThe residue was purified by column chromatography on silica gel
9. customthe eluate with ethyl acetate-hexane (1:8) was collected

ORD record

ord-744e1d3b98034be08859ff4b995b91c8

Source dataset

uspto-grants-2005_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06949585B2