Methanol → HCID 59625678, Verbindung

HRID 468088

Reaktionsgleichung

Reaktionsgleichung von HRID 468088
C([N:14]1[CH2:17][CH:16]([N:18]2[CH2:23][CH2:22][N:21]([C:24](=[O:29])[C:25]([F:28])([F:27])[F:26])[CH2:20][CH2:19]2)[CH2:15]1)(C1C=CC=CC=1)C1C=CC=CC=1.ClC(OC(Cl)C)=O.CO.CCOCC>C(Cl)Cl>[NH:14]1[CH2:15][CH:16]([N:18]2[CH2:19][CH2:20][N:21]([C:24](=[O:29])[C:25]([F:26])([F:27])[F:28])[CH2:22][CH2:23]2)[CH2:17]1

Komponenten

6

Edukt 4

HCID 887MethanolHCID 3283Diethyl EtherHCID 5213051-Chloroethyl chloroformateHCID 596259751-[4-(1-Benzhydryl-azetidin-3-yl)-piperazin-1-yl]-2,2,2-trifluoro-ethanone

Produkt 1

HCID 59625678HCID 59625678, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To a solution of compound 1f (2.11 g, 5.23 mmol) in CH2Cl2 (60 mL) was added 1-chloroethyl chloroformate (2.0 mL, 18.35 mmol) at 0° C. under N2. The mixture was stirred at 0° C. for 90 min and then MeOH (4 mL) was added. The mixture was refluxed for 1 h. Upon cooling, Et2O (50 mL) was added to the mixture. The resulting solid was collected by filtration and dried. The crude compound 1g was used in the next reaction without further purification. MS m/z (M+H+) 238.1.

Aufarbeitung

  1. temperatureThe mixture was refluxed for 1 h
  2. temperatureUpon cooling
  3. filtrationThe resulting solid was collected by filtration
  4. customdried
  5. customThe crude compound 1g was used in the next reaction without further purification

Quellen und Nachweise

ORD-Eintrag
ord-aae40ac31f8a4793ad6491f3954cb28a
Quelldatensatz
uspto-grants-2014_01
Patentnummer
US08623858B2

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