Hydrochloric Acid → HCID 19973181, Verbindung

HRID 1901288Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1901288
CC([N:5]([CH2:9][C:10]([NH:12][N:13]1[CH:17]=[CH:16][CH:15]=[C:14]1[C:18](=[O:20])[CH3:19])=[O:11])C(=O)[O-])(C)C.[ClH:21].CCOC(C)=O.CCCCCC>C(OCC)(=O)C.C(O)(C)C>[ClH:21].[C:18]([C:14]1[N:13]([NH:12][C:10](=[O:11])[CH2:9][NH2:5])[CH:17]=[CH:16][CH:15]=1)(=[O:20])[CH3:19]

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 21226206Ethyl acetate hexaneHCID 867474421,1-dimethylethyl-[2-[(2-acetyl-1H-pyrrol-1-yl)amino]-2-oxoethyl]carbamate

Produkt 1

HCID 19973181HCID 19973181, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3776IsopropanolLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a stirred solution consisting of 1,1-dimethylethyl-[2-[(2-acetyl-1H-pyrrol-1-yl)amino]-2-oxoethyl]carbamate (5.90 g) in ethyl acetate (45 ml) and isopropanol (35ml) was added ethereal HCl (1.7M, excess). The resulting suspension was gently heated until the reaction mixture was homogeneous. After stirring for 24 hours at room temperature, the reaction appeared complete by TLC (silica gel, 50% EtOAc/hexane). The solid product was collected by filtration under nitrogen and recrystallized from methanol/ether to afford 3.30 g of the product, m.p. 179°-182° C.

Aufarbeitung

  1. temperatureThe resulting suspension was gently heated until the reaction mixture
  2. filtrationThe solid product was collected by filtration under nitrogen
  3. customrecrystallized from methanol/ether

Quellen und Nachweise

ORD-Eintrag
ord-2c00d0da6fa8482a8f73803d2b689126
Quelldatensatz
uspto-grants-1996_11
Patentnummer
US05576446

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