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Hydrochloric Acid → [4-Cyano-2,3-bis-[(2-methoxy-ethoxy)-methoxy]-phenyl]bromoacetic acid

HRID 2576
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2576
[CH:1]([Br:4])(Br)Br.[Br-].[Li+].[OH-:7].[K+].[C:9]([C:11]1[CH:18]=[CH:17][C:14](C=O)=[C:13]([O:19][CH2:20][O:21][CH2:22][CH2:23][O:24][CH3:25])[C:12]=1[O:26][CH2:27][O:28][CH2:29][CH2:30][O:31][CH3:32])#[N:10].Cl.[O:34]1[CH2:39]COCC1>C(OCC)(=O)C.O>[C:9]([C:11]1[CH:18]=[CH:17][C:14]([CH:1]([Br:4])[C:39]([OH:34])=[O:7])=[C:13]([O:19][CH2:20][O:21][CH2:22][CH2:23][O:24][CH3:25])[C:12]=1[O:26][CH2:27][O:28][CH2:29][CH2:30][O:31][CH3:32])#[N:10]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 6

HCID 313Hydrochloric AcidHCID 5558BromoformHCID 14797Potassium HydroxideHCID 312751,4-DioxaneHCID 82050Lithium BromideHCID 183590784-Cyano-2,3-bis-[(2-methoxy-ethoxy)-methoxy]-benzaldehyde

Produkt 1

HCID 18359186
[4-Cyano-2,3-bis-[(2-methoxy-ethoxy)-methoxy]-phenyl]bromoacetic acid

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

440 microliters of bromoform were added at -5° C. to a mixture of 4.26 mg of lithium bromide, 598 mg of potassium hydroxide and 5 ml of water and then, a solution of 825 mg of a 4-cyano-2,3-bis-[(2-methoxy-ethoxy)-methoxy]-benzaldehyde (preparation given hereafter) in 5 ml of dioxane was added dropwise. The mixture was stirred for 72 hours at 0° C. to -5° C. and was poured into a stirred mixture at 0° C. to -5° C. of 15 ml of ethyl acetate and 11 ml of hydrochloric acid. Extraction was carried out with ethyl acetate and the extracts were washed, dried and evaporated to dryness under reduced pressure. The oil obtained was used as is for the following step.

Aufarbeitung

  1. extractionExtraction
  2. washthe extracts were washed
  3. customdried
  4. customevaporated to dryness under reduced pressure
  5. customThe oil obtained

Quellen und Nachweise

ORD-Eintrag
ord-a2d6a5f5e06e41cb9bec46be781f750a
Quelldatensatz
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05728828

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