Methanol → HCID 59625678, Verbindung

HRID 1911099

Reaktionsgleichung

Reaktionsgleichung von HRID 1911099
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-e527049969ac4bbb9818c629d2bcc86d
Quelldatensatz
uspto-grants-2013_12
Patentnummer
US08604017B2

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