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Sodium Hydroxide → HCID 86648131, Verbindung

HRID 2388247
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2388247
[OH-:1].[Na+].Cl.[NH2:4]O.[CH2:6]([O:8][C:9](=[O:18])[C:10](=[O:17])[CH:11]([CH3:16])[C:12](=O)[CH2:13][CH3:14])[CH3:7]>O>[CH2:6]([O:8][C:9](=[O:18])[C:10](=[O:17])[CH:11]([CH3:16])[C:12](=[N:4][OH:1])[CH2:13][CH3:14])[CH3:7]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 3017239Ethyl 3-methyl-2,4-dioxohexanoate

Produkt 1

HCID 86648131HCID 86648131, VerbindungAusbeute 53,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Sodium hydroxide (1.58 g, 39.4 mmol) was dissolved in 8.5 mL of water. Hydroxylamine hydrochloride (2.74 g, 39.4 mmol) was added and the reaction mixture was stirred until complete dissolution was achieved. 3-Methyl-2,4-dioxo-hexanoic acid ethyl ester (6.37 g, 34.2 mmol) was added and the resulting mixture was stirred at ambient temperature for 16 h. The reaction mixture was extracted with EtOAc (3×50 mL) and the organic layers were combined, dried over MgSO4 and concentrated. The crude oil was purified by chromatography (0-40% EtOAc/hexanes) to give 3.7 g of the title compound. MS: (+) m/z 202.35 (M+1).

Aufarbeitung

  1. stirringthe resulting mixture was stirred at ambient temperature for 16 h
  2. extractionThe reaction mixture was extracted with EtOAc (3×50 mL)
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated
  5. customThe crude oil was purified by chromatography (0-40% EtOAc/hexanes)

Quellen und Nachweise

ORD-Eintrag
ord-255dcc25df634218abac8988b00c4f94
Quelldatensatz
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08269008B2

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