HCID 18368343, Verbindung → HCID 9884882, Verbindung

HRID 379696Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 379696
C(OC([NH:8][CH2:9][CH2:10][O:11][C:12]1[CH:30]=[CH:29][C:15]([NH:16][C:17](=[O:28])[C:18]2[C:23]([O:24][CH3:25])=[CH:22][CH:21]=[CH:20][C:19]=2[O:26][CH3:27])=[CH:14][CH:13]=1)=O)(C)(C)C.Cl.O1CCOCC1>>[NH2:8][CH2:9][CH2:10][O:11][C:12]1[CH:30]=[CH:29][C:15]([NH:16][C:17](=[O:28])[C:18]2[C:19]([O:26][CH3:27])=[CH:20][CH:21]=[CH:22][C:23]=2[O:24][CH3:25])=[CH:14][CH:13]=1

Komponenten

3

Edukt 2

HCID 18368343HCID 18368343, VerbindungHCID 204431481,4-Dioxane hydrochloride

Produkt 1

HCID 9884882HCID 9884882, VerbindungAusbeute 83,3 %

Versuchsvorschrift

4′-[2-(tert-Butoxycarbonylamino)ethoxy]-2,6-dimethoxybenzanilide (1.17 g) was added with 4N HCl/dioxane (5 ml) and mixed for 6 hours at room temperature. The reaction mixture was concentrated under vacuum and residue was dissolved into chloroform (50 ml). The solution was washed with 1N sodium hydroxide aqueous solution (10 ml) followed by saturated sodium chloride (20 ml). After concentration under vacuum to small volume, the solution was subjected to purification by silica-gel column chromatography (chloroform methanol=4:1) to obtain 4′-(2-aminoethoxy)-2,6-dimethoxybenzanilide (0.74 g) as white powder.

Aufarbeitung

  1. additionmixed for 6 hours at room temperature
  2. concentrationThe reaction mixture was concentrated under vacuum and residue
  3. dissolutionwas dissolved into chloroform (50 ml)
  4. washThe solution was washed with 1N sodium hydroxide aqueous solution (10 ml)
  5. concentrationAfter concentration under vacuum to small volume
  6. customthe solution was subjected to purification by silica-gel column chromatography (chloroform methanol=4:1)

Quellen und Nachweise

ORD-Eintrag
ord-99ba9c1f3c4f480ea9a3c9bb1a06c07d
Quelldatensatz
uspto-grants-2001_10
Patentnummer
US06300368B1

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