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Potassium bisulfate → HCID 88414407, Verbindung

HRID 1963087
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1963087
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]([C:16]2[N:20]3[N:21]=[CH:22][C:23]([C:25](=[O:30])N(OC)C)=[CH:24][C:19]3=[C:18]([C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=3)[C:17]=2[CH2:37][C:38]2[CH:43]=[CH:42][CH:41]=[C:40]([F:44])[C:39]=2[CH3:45])=[O:15])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[H-].C(O[Al](OC(C)(C)C)OC(C)(C)C)(C)(C)C.[Li+].S([O-])(O)(=O)=O.[K+]>C1COCC1>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH2:10][N:11]([C:14]([C:16]2[N:20]3[N:21]=[CH:22][C:23]([CH:25]=[O:30])=[CH:24][C:19]3=[C:18]([C:31]3[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=3)[C:17]=2[CH2:37][C:38]2[CH:43]=[CH:42][CH:41]=[C:40]([F:44])[C:39]=2[CH3:45])=[O:15])[CH2:12][CH2:13]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 516920Potassium bisulfateHCID 16710494Lithium tri-tert-butoxyaluminohydrideHCID 88414359HCID 88414359, Verbindung

Produkt 1

HCID 88414407HCID 88414407, VerbindungAusbeute 40,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Reaktionsbedingungen

Temperatur
2.5 °C

Versuchsvorschrift

To a solution of the compound of step 1 (0.990 g, 1.61 mmol) in 11 ml of anhydrous THF, cooled to 0° C. under an atmosphere of nitrogen, was added a 1 M solution of lithium tri-tert-butoxy-aluminium hydride in THF. The mixture was stirred at 0-5° C. for 3.5 h. Then a 0.5 M aqueous solution of potassium hydrogensulfate (20 ml) was added, the mixture was vigorously stirred for 1 min and then extracted twice with EA (30 ml). The combined organic phases were washed with a saturated solution of sodium hydrogencarbonate (20 ml) and brine (40 ml), dried over magnesium sulfate and evaporated to dryness. The residue was purified by chromatography on silica gel (cyclohexane/EA, 70:30, then 65:35) to give 0.363 g of the title compound as a yellow solid melting at 208-209° C.

Aufarbeitung

  1. stirringthe mixture was vigorously stirred for 1 min
  2. extractionextracted twice with EA (30 ml)
  3. washThe combined organic phases were washed with a saturated solution of sodium hydrogencarbonate (20 ml) and brine (40 ml)
  4. dry with materialdried over magnesium sulfate
  5. customevaporated to dryness
  6. customThe residue was purified by chromatography on silica gel (cyclohexane/EA, 70:30

Quellen und Nachweise

ORD-Eintrag
ord-e8daa694b31449dfa071731370f81afd
Quelldatensatz
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08415336B2

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