Sodium Hydroxide → HCID 21955005, Verbindung

HRID 254936Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 254936
[N:1]1([C:7]([C:9]2[CH:14]=[C:13]([C:15]([F:18])([F:17])[F:16])[CH:12]=[C:11]([N+:19]([O-:21])=[O:20])[CH:10]=2)=O)[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[Na+]>C1COCC1>[N+:19]([C:11]1[CH:10]=[C:9]([CH:14]=[C:13]([C:15]([F:18])([F:17])[F:16])[CH:12]=1)[CH2:7][N:1]1[CH2:2][CH2:3][O:4][CH2:5][CH2:6]1)([O-:21])=[O:20]

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 219549894-(3-Nitro-5-trifluoromethyl-benzoyl)-morpholine

Produkt 1

HCID 21955005HCID 21955005, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

To a solution of morpholin-4-yl-(3-nitro-5-(trifluoromethyl)phenyl)methanone (304 mg, 1.0 mmol) in 15 mL of THF was added lithium aluminum hydride (152 mg, 4 mmol) in THF (7 mL) under nitrogen. The dark colored solution was refluxed for 2 hours and then cooled. NaOH solution was added (0.5 N, 15 mL) dropwise. The basic solution was washed with methylene chloride (3×40 mL) and the pooled organic layers were washed with HCl solution (5%). The aqueous layer was separated, basified with NaOH to pH 8, and extracted with ethyl acetate. The ethyl acetate solution was dried over anhydrous Na2SO4. The solution was used in further reactions without further work-up.

Aufarbeitung

  1. temperatureThe dark colored solution was refluxed for 2 hours
  2. temperaturecooled
  3. washThe basic solution was washed with methylene chloride (3×40 mL)
  4. washthe pooled organic layers were washed with HCl solution (5%)
  5. customThe aqueous layer was separated
  6. extractionextracted with ethyl acetate
  7. dry with materialThe ethyl acetate solution was dried over anhydrous Na2SO4

Quellen und Nachweise

ORD-Eintrag
ord-3d53a97ccdf04034aec3b043dc5fa03d
Quelldatensatz
uspto-grants-2011_01
Patentnummer
US07875728B2

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