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

HRID 1418781Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1418781
[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]

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-a20ba5f99b09448abadf7af1e5f1f809
Quelldatensatz
uspto-grants-1999_03
Patentnummer
US05883248

Notizen zur Reaktion

Wird geladen…