Water → HCID 69300599, Verbindung

HRID 2196531Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2196531
[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]1[N:10]([C:11]2[CH:12]=[C:13]([CH:16]=[CH:17][CH:18]=2)[C:14]#[N:15])[N:9]=[C:8]([C:19]([F:22])([F:21])[F:20])[CH:7]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>C1COCC1>[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]1[N:10]([C:11]2[CH:12]=[C:13]([CH2:14][NH2:15])[CH:16]=[CH:17][CH:18]=2)[N:9]=[C:8]([C:19]([F:21])([F:20])[F:22])[CH:7]=1

Komponenten

6

Edukt 4

HCID 962Water2×HCID 14798Sodium HydroxideHCID 158809863-[3-(Trifluoromethyl)-5-(2-furanyl)-1H-pyrazole-1-yl]benzonitrileHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 69300599HCID 69300599, VerbindungAusbeute 100 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a stirred solution of 53 (3 g, 9.89 mmol) in THF (50 mL) at 0° C. was added lithium aluminium hydride (0.939 g, 24.73 mmol). The resulting suspension was allowed to stir for 0.5 h. The reaction mixture was then warmed to room temperature and stirred for another 1 h. The following was added sequentially: 0.9 mL of water, 0.9 mL of 15% NaOH and 1.8 mL of water. The white solid was removed by filtration and the filtrate evaporated under vacuum. The title product 54 (3.04 g, 100% yield) was isolated as a pale yellow oil. Crude was used without any further purification. LRMS (ESI): calc. 307.3; found 308.4 (MH)+.

Aufarbeitung

  1. stirringstirred for another 1 h
  2. additionThe following was added sequentially
  3. customThe white solid was removed by filtration
  4. customthe filtrate evaporated under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-7c3ac86c7c5f4d36a3db2df3297dfda9
Quelldatensatz
uspto-grants-2012_12
Patentnummer
US08338437B2

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