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Sodium Hydroxide → 5-Phenyl-[1,4]diazepane

HRID 1637166
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1637166
[H-].[H-].[H-].[H-].[Li+].[Al+3].[C:7]1([CH:13]2[NH:19][CH2:18][CH2:17][NH:16][C:15](=O)[CH2:14]2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[OH-].[Na+]>C1COCC1.O>[C:7]1([CH:13]2[NH:19][CH2:18][CH2:17][NH:16][CH2:15][CH2:14]2)[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 14798Sodium HydroxideHCID 130482357-Phenyl-1,4-diazepan-5-oneHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 193479295-Phenyl-[1,4]diazepaneAusbeute 105,8 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel3×
HCID 8028
Tetrahydrofuran
Lösungsmittel

Versuchsvorschrift

2.0 g LiAlH4 were suspended in THF under a nitrogen atmosphere, and then 5.0 g hexahydro-7-phenyl-1,4-diazepin-5-one were added thereto at 10° C. Then the mixture was stirred for 8 hours at room temperature. Under a nitrogen atmosphere, 5 ml water, 2.2 g NaOH, dissolved in 5 ml water, and again 3 ml water were then added dropwise in succession, and the mixture was stirred for 15 minutes at room temperature. Once the resulting salts had been filtered out, the filtrate was reduced to dryness under vacuum. 4.9 g of 7-phenyl-1,4-diazepane were obtained, which was reacted without further purification.

Aufarbeitung

  1. customat 10° C
  2. stirringthe mixture was stirred for 15 minutes at room temperature
  3. filtrationOnce the resulting salts had been filtered out

Quellen und Nachweise

ORD-Eintrag
ord-667d7ebca57e4a919e0a31c6a303371c
Quelldatensatz
uspto-grants-2000_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06040303

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