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Hydroxylamine, O-(3-chloro-2-propenyl)-, hydrochloride → HCID 178449940, Verbindung

HRID 2308578
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2308578
C[O-].[Na+].Cl.[Cl:5][CH:6]=[CH:7][CH2:8][O:9][NH2:10].[C:11]([CH:16]1[C:21](=[O:22])[CH2:20][CH:19]([CH2:23][CH:24]([S:26][CH2:27][CH3:28])[CH3:25])[CH2:18][C:17]1=[O:29])(=O)[CH2:12][CH2:13][CH3:14]>CO>[Cl:5][CH:6]=[CH:7][CH2:8][O:9][N:10]=[C:11]([C@H:16]1[C:21](=[O:22])[CH2:20][C@H:19]([CH2:23][CH:24]([S:26][CH2:27][CH3:28])[CH3:25])[CH2:18][C:17]1=[O:29])[CH2:12][CH2:13][CH3:14]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 158057Hydroxylamine, O-(3-chloro-2-propenyl)-, hydrochlorideHCID 28347542-Butyryl-5-[2-(ethylthio)propyl]-1,3-cyclohexanedioneHCID 10942334Sodium Methoxide

Produkt 1

HCID 178449940HCID 178449940, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

0.38 g of sodium methoxide, 10 ml of methanol, and 1.0 g of 3-chloroallyloxyamine hydrochloride (H2NOCH2CH=CHCl) were admixed together and then stirred for 10 minutes at room temperature. 2 g of 2-butyryl-5-(2-ethylthiopropyl)cyclohexane-1,3-dione was added and the resulting mixture stirred for about two days at room temperature. The mixture was then concentrated by evaporation and the concentrate mixed with 60 ml of diethyl ether and 40 ml of water. The ether layer was extracted with 40 ml of aqueous 2 wt. % sodium hydroxide solution, washed with 20 ml of water, dried over anhydrous magnesium sulfate and evaporated affording a minor amount of the title compound as the trans isomer.

Aufarbeitung

  1. stirringthe resulting mixture stirred for about two days at room temperature
  2. concentrationThe mixture was then concentrated by evaporation
  3. additionthe concentrate mixed with 60 ml of diethyl ether and 40 ml of water
  4. extractionThe ether layer was extracted with 40 ml of aqueous 2 wt. % sodium hydroxide solution
  5. washwashed with 20 ml of water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-f14811ed5d074a11a7ea681453140aa3
Quelldatensatz
uspto-grants-1987_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
USRE032489

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