Tetrahydrofuran → HCID 44224242, Verbindung

HRID 76941Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 76941
[CH3:1][N:2]([CH3:31])[C:3]1([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH2:8][CH2:7][C:6]([N:15]([CH3:24])[C:16](=O)[C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH2:5][CH2:4]1.C1COCC1.[H-].[H-].[H-].[H-].[Li+].[Al+3]>O>[CH2:16]([N:15]([CH3:24])[C:6]1([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH2:7][CH2:8][C:3]([N:2]([CH3:31])[CH3:1])([C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)[CH2:4][CH2:5]1)[C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1

Komponenten

5

Edukt 3

HCID 8028Tetrahydrofuran2×HCID 21226445Aluminium lithium hydrideHCID 68631670N-(4-dimethylamino-1,4-diphenyl-cyclohexyl)-N-methyl-benzamide

Produkt 1

HCID 44224242HCID 44224242, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

The title compound from step 1 (160 mg, 0.387 mmol) was dissolved in abs. THF (15 mL) and mixed with LiAlH4 (29 mg, 0.775 mmol) in argon. The batch was boiled for 7 h with reflux and then cooled to room temperature. THF (5 mL) and H2O (5 mL) were added to the batch with ice cooling and subsequently stirred for 30 min. The batch was filtered over a fitted glass filter with diatomaceous earth and subsequently rinsed with dichloromethane (50 mL). The combined filtrates were concentrated to low volume in vacuum.

Aufarbeitung

  1. temperaturewith reflux
  2. filtrationThe batch was filtered over a fitted glass
  3. filtrationfilter with diatomaceous earth
  4. washsubsequently rinsed with dichloromethane (50 mL)
  5. concentrationThe combined filtrates were concentrated to low volume in vacuum

Quellen und Nachweise

ORD-Eintrag
ord-58d69b55385c40fcb60021d230136f8b
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08835689B2

Notizen zur Reaktion

Wird geladen…