Hydrochloric Acid → HCID 19091987, Verbindung

HRID 487526

Reaktionsgleichung

Reaktionsgleichung von HRID 487526
[CH2:1]([OH:3])[CH3:2].Cl[S:5]([CH:8]([CH2:11][CH3:12])[CH2:9]Cl)(=[O:7])=[O:6].[NH2:13][C:14]1[CH:27]=[CH:26][C:17]([C:18]([CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22])=[O:19])=[CH:16][CH:15]=1.Cl.CN(C)C(=[O:33])C>N1C=CC=CC=1.O1CCCC1>[CH2:1]([O:3][C:9]([CH:8]([S:5]([NH:13][C:14]1[CH:15]=[CH:16][C:17]([C:18]([CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22])=[O:19])=[CH:26][CH:27]=1)(=[O:7])=[O:6])[CH2:11][CH3:12])=[O:33])[CH3:2]

Komponenten

8

Edukt 5

HCID 313Hydrochloric AcidHCID 702EthanolHCID 31374DimethylacetamideHCID 3045879Acetic acid, (p-aminobenzoyl)-, ethyl ester (6CI,7CI)HCID 12589201HCID 12589201, Verbindung

Produkt 1

HCID 19091987HCID 19091987, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1049PyridineLösungsmittelHCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

Ethanol (3.6 g) and tetrahydrofuran (10 ml) were dropwise added to a solution of 2-chlorosulfonylbutyl chloride (14.4 g) and tetrahydrofuran (21 ml) while cooling with ice. After stirring at room temperature for 1 hour, ethyl p-aminobenzoylacetate (13.3 g), N,N-dimethylacetamide (33 ml) and pyridine (12.2 g) were added thereto, and the mixture was heated for refluxing for 30 minutes. 0.5 N hydrochloric acid (30 ml) was added to the reaction solution, and the mixture was extracted with ethyl acetate (120 ml). The extracted solution was washed with a sodium chloride aqueous solution (120 ml), then dried over magnesium sulfate, and concentrated. An oily product, ethyl p-(1-ethoxycarbonylpropanesulfonamido)benzoylacetate was quantitatively obtained.

Aufarbeitung

  1. temperaturewhile cooling with ice
  2. temperaturethe mixture was heated
  3. temperaturefor refluxing for 30 minutes
  4. extractionthe mixture was extracted with ethyl acetate (120 ml)
  5. washThe extracted solution was washed with a sodium chloride aqueous solution (120 ml)
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-dddf2d00a6de4b4c9a4eaf8c36c60901
Quelldatensatz
uspto-grants-1994_03
Patentnummer
US05296344

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