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

HRID 428833Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 428833
[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 here-after) 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-b19382322eee470db0fdeb7fa38d1206
Quelldatensatz
uspto-grants-2001_11
Patentnummer
US06313305B1

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