Triethylamine → t-Butyl 4-(4-methoxycarbonylbenzoyl)piperazine-1-carboxylate

HRID 747682

Reaktionsgleichung

Reaktionsgleichung von HRID 747682
[N:1]1([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.C(N(CC)CC)C.[Cl-].[C:22]([O:33][CH3:34])(=[O:32])[C:23]1[CH:31]=[CH:30][C:26]([C:27]([O-])=[O:28])=[CH:25][CH:24]=1>CN(C)C=O.Cl>[CH3:34][O:33][C:22]([C:23]1[CH:31]=[CH:30][C:26]([C:27]([N:4]2[CH2:5][CH2:6][N:1]([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[CH2:2][CH2:3]2)=[O:28])=[CH:25][CH:24]=1)=[O:32]

Komponenten

6

Edukt 3

HCID 8471TriethylamineHCID 143452tert-Butyl piperazine-1-carboxylateHCID 22493623Monomethyl terephthalate chloride

Produkt 1

HCID 17789205t-Butyl 4-(4-methoxycarbonylbenzoyl)piperazine-1-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 313Hydrochloric AcidLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

4.93 g (26.5 mmol) of t-butyl piperazine-1-carboxylate and 4.8 ml (34.5 mmol) of triethylamine were stirred in 50 ml of dimethylformamide under cooling with ice. 5.25 g (26.5 mmol) of monomethyl terephthalate chloride was slowly added to the resultant mixture, and they were stirred for 16 hours. The temperature was elevated to room temperature, and the reaction liquid was diluted with 1 N hydrochloric acid. After the extraction with ethyl acetate followed by the treatment in an ordinary manner, the title compound was obtained.

Aufarbeitung

  1. temperatureunder cooling with ice
  2. customwas elevated to room temperature
  3. customthe reaction liquid
  4. extractionAfter the extraction with ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-f920af3f16aa4415b543e2effaf1a3a1
Quelldatensatz
uspto-grants-2008_07
Patentnummer
US07396844B1

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