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Hydrochloric Acid → HCID 21317568, Verbindung

HRID 328800
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 328800
[H-].[Na+].[CH3:3][O:4][C:5](=[O:21])[CH:6]([S:17]([CH3:20])(=[O:19])=[O:18])[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]([O:15][CH3:16])=[O:14].[H][H].I[CH2:25][CH2:26][CH2:27][CH:28]([O:41][C:42](=[O:44])[CH3:43])[CH2:29][O:30][C:31]1[CH:36]=[CH:35][CH:34]=[C:33]([C:37]([F:40])([F:39])[F:38])[CH:32]=1.Cl>CN(C)C=O.O.CCOCC>[CH3:20][S:17]([C:6]([C:5]([O:4][CH3:3])=[O:21])([CH2:25][CH2:26][CH2:27][CH:28]([O:41][C:42](=[O:44])[CH3:43])[CH2:29][O:30][C:31]1[CH:36]=[CH:35][CH:34]=[C:33]([C:37]([F:39])([F:40])[F:38])[CH:32]=1)[CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]([O:15][CH3:16])=[O:14])(=[O:19])=[O:18]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 5

HCID 313Hydrochloric AcidHCID 24758Sodium hydrideHCID 21317577HCID 21317577, VerbindungHCID 54054723Dimethyl-2-methylsulfonylazelateHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 21317568HCID 21317568, VerbindungAusbeute 88 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 3283Diethyl EtherLösungsmittelHCID 6228DimethylformamideLösungsmittel3×

Reaktionsbedingungen

Temperatur
5 °C

Versuchsvorschrift

A 50% oil dispersion of sodium hydride (2.11 g., 0.044 mole) in mineral oil is washed with petroleum ether and then suspended in dry dimethylformamide (30 ml.) under a nitrogen atmosphere at room temperature. To this suspension is added a solution of dimethyl-2-methylsulfonyl-azelate (11.8 g., 0.04 mole) in dry dimethylformamide (30 ml.). After the evolution of hydrogen is completed, the mixture is cooled to 5° C. in an ice bath and a solution of 1-iodo-4-acetoxy-5-(3-trifluoromethylphenoxy)pentane (18.3 g., 0.044 mole) in dry dimethylformamide (30 ml.) is added dropwise. After 48 hours, ether is added to the reaction mixture to precipitate sodium iodide which is removed by filtration. The filtrate is concentrated in vacuo to give a residue which is diluted with water, acidified with 6N hydrochloric acid, and extracted with ether. The ether extracts are washed with water until neutral, dried over anhydrous magensium sulfate, and concentrated in vacuo to give the title compound (20.5 g., 0.035 mole, 88%).

Aufarbeitung

  1. customto precipitate sodium iodide which
  2. customis removed by filtration
  3. concentrationThe filtrate is concentrated in vacuo
  4. customto give a residue which
  5. extractionextracted with ether
  6. washThe ether extracts are washed with water until neutral,
  7. dry with materialdried over anhydrous magensium sulfate
  8. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-02865890d17948a892b135542e046d54
Quelldatensatz
uspto-grants-1977_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04018802

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