Pyridine → HCID 13728618, Verbindung

HRID 1365926Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1365926
ClC(Cl)(OC(=O)[O:6][C:7]([Cl:10])(Cl)Cl)Cl.[N:13]1([C:19](=[O:21])[CH3:20])[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1.N1C=CC=CC=1>C(Cl)Cl>[C:19]([N:13]1[CH2:18][CH2:17][N:16]([C:7]([Cl:10])=[O:6])[CH2:15][CH2:14]1)(=[O:21])[CH3:20]

Komponenten

5

Edukt 3

HCID 1049PyridineHCID 837951-AcetylpiperazineHCID 94429Triphosgene

Produkt 1

HCID 13728618HCID 13728618, VerbindungAusbeute 75,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

To a stirred solution of carbonic acid ditrichloromethyl ester (triphosgene) (2.31 g, 7.80 mmol) in CH2Cl2 (30 ml) at 0° C., was added a solution of 1-piperazin-1-yl-ethanone (2.0 g, 15.6 mmol) and pyridine (1.38 ml, 17.2 mmol) in CH2Cl2 (5 ml) over 30 minutes. The temperature was raised to RT, and stirring was continued over night. The organic phase was washed with H2O, dried over Na2SO4. Purification by flash chromatography (SiO2, EtOAc) yielded 1.12 g (38%) of the title compound as white solid.

Aufarbeitung

  1. waitwas continued over night
  2. washThe organic phase was washed with H2O
  3. dry with materialdried over Na2SO4
  4. customPurification by flash chromatography (SiO2, EtOAc)

Quellen und Nachweise

ORD-Eintrag
ord-eb8f9433419340aabce7de6f558a7303
Quelldatensatz
uspto-grants-2011_02
Patentnummer
US07893062B2

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