Hydrochloric Acid → HCID 15341788, Verbindung

HRID 1033619Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1033619
[OH:1][C:2]1[C:11]([CH2:12][CH:13]=[CH2:14])=[C:10]([OH:15])[CH:9]=[CH:8][C:3]=1[C:4](OC)=[O:5].[CH3:16][NH2:17].[Cl-].[NH4+].Cl>>[OH:1][C:2]1[C:11]([CH2:12][CH:13]=[CH2:14])=[C:10]([OH:15])[CH:9]=[CH:8][C:3]=1[C:4]([NH:17][CH3:16])=[O:5]

Komponenten

5

Edukt 4

HCID 313Hydrochloric AcidHCID 6329MethylamineHCID 25517Ammonium ChlorideHCID 13019279Methyl 2,4-dihydroxy-3-(prop-2-en-1-yl)benzoate

Produkt 1

HCID 15341788HCID 15341788, VerbindungAusbeute 75 %

Versuchsvorschrift

the compound of Example 5 (3.5 g) and excess methyl amine 40% aqueous solution) were stirred overnight at 50° C. in the presence of a few crystals of ammonium chloride. The reaction mixture was cooled and neutralized with 10% hydrochloric acid then extracted with ethyl acetate. The organic layer was dried over magnesium sulfate and concentrated under vacuum. The crude crystals were dissolved in chloroform and then hexane was added until the product precipitated out of solution. The precipitate was filtered and dried to give the product (2.5 g, 75% yield).

Aufarbeitung

  1. temperatureThe reaction mixture was cooled
  2. extractionthen extracted with ethyl acetate
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. concentrationconcentrated under vacuum
  5. dissolutionThe crude crystals were dissolved in chloroform
  6. additionhexane was added until the product
  7. customprecipitated out of solution
  8. filtrationThe precipitate was filtered
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-9fa2d9393d3a465bb68d3dd456b1ab21
Quelldatensatz
uspto-grants-1994_05
Patentnummer
US05310951

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