Potassium sodium tartarate → HCID 22005358, Verbindung

Reaktionsgleichung

[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[C:12]([CH:19]([CH3:21])[CH3:20])[N:11]=[C:10]([O:22][CH3:23])[C:9]=2[C:24](OC)=[O:25])=[CH:4][CH:3]=1.[H-].C([Al+]CC(C)C)C(C)C.C(C(C(C([O-])=O)O)O)([O-])=O.[Na+].[K+]>C1(C)C=CC=CC=1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[C:12]([CH:19]([CH3:21])[CH3:20])[N:11]=[C:10]([O:22][CH3:23])[C:9]=2[CH2:24][OH:25])=[CH:6][CH:7]=1

Komponenten

Reaktionsbedingungen

Temperatur: -78 °C

Versuchsvorschrift

1.48 g (3.95 mmol) of the compound from Example 5 are dissolved in 30 ml of toluene, the solution is cooled to -78° C. under nitrogen and 6.6 ml (10 mmol) of a 1.5 molar solution of diisobutylaluminium hydride in toluene are added dropwise at this temperature. The cooling bath is removed and the mixture is stirred at room temperature for 2 h. After hydrolysis using 20% strength aqueous potassium sodium tartrate solution, the organic phase is separated off, the aqueous phase is washed three times with toluene, and the combined organic phases are washed with saturated sodium chloride solution and dried using sodium sulphate.

Aufarbeitung

customThe cooling bath is removed
customAfter hydrolysis
customthe organic phase is separated off
washthe aqueous phase is washed three times with toluene
washthe combined organic phases are washed with saturated sodium chloride solution
customdried

Quellen und Nachweise

ORD-Eintrag: ord-0cdd43d2293f4b07afd31b99a9d6e306
Quelldatensatz: uspto-grants-1995_05
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US05418243

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