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Potassium sodium tartarate → HCID 67056312, Verbindung

HRID 714645
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 714645
[F:1][C:2]([F:20])([F:19])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[CH:10]=[C:11]([CH:16]=[CH:17][N:18]=1)[C:12](OC)=[O:13].[H-].[Al+3].[Li+].[H-].[H-].[H-].C(C(C(C([O-])=O)O)O)([O-])=O.[K+].[Na+]>C1COCC1>[F:19][C:2]([F:1])([F:20])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[CH:10]=[C:11]([CH2:12][OH:13])[CH:16]=[CH:17][N:18]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 9855836Potassium sodium tartarateHCID 21226445Aluminium lithium hydrideHCID 67396524HCID 67396524, Verbindung

Produkt 1

HCID 67056312HCID 67056312, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

432 mg (1.54 mmol) of the compound from Example 58A were dissolved in 10 ml of THF, and 1.08 ml (1.08 mmol) of a 1 M solution of lithium aluminum hydride in THF were added at −10° C. After the addition had ended, the mixture was stirred at RT for 2 h. For work-up, 4 ml of a saturated sodium potassium tartrate solution were added at RT, and the mixture was extracted with 15 ml of ethyl acetate. The organic phase was washed once with 10 ml of saturated sodium potassium tartrate solution, dried over magnesium sulfate, filtered and concentrated under reduced pressure. This gave 497 mg (>100% of theory) of the target compound which were reacted further without any further purification.

Aufarbeitung

  1. additionAfter the addition
  2. extractionthe mixture was extracted with 15 ml of ethyl acetate
  3. washThe organic phase was washed once with 10 ml of saturated sodium potassium tartrate solution
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThis gave 497 mg (>100% of theory) of the target compound which were reacted further without any further purification

Quellen und Nachweise

ORD-Eintrag
ord-415161255ab148c5b224d675d6e329b8
Quelldatensatz
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09187466B2

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