1-Methoxy-2-propanol → HCID 17750604, Verbindung

HRID 333930

Reaktionsgleichung

Reaktionsgleichung von HRID 333930
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=[C:4]([CH3:12])[CH:3]=1.COCC(O)C.[N:19]1([C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1>>[CH3:12][C:4]1[CH:3]=[C:2]([N:22]2[CH2:21][CH2:20][N:19]([C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[CH2:24][CH2:23]2)[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=1

Komponenten

4

Versuchsvorschrift

4-Chloro-2-methylquinoline (5 g, 28 mmol) was mixed with 1-methoxy-2-propanol, tert-butyl piperazine-1-carboxylate was added (5.74 g, 30.8 mmol) and the mixture was refluxed for 4.5 hours after which the product started to precipitate. The mixture was concentrated under reduced pressure and left at room temperature for 48 hours. The product was separated by filtration, washed with ethylacetate and dried at 50° C. 4.382 g of a solid were obtained (13.38 mmol, 48%). MS (APCI): m/z=327.9 [M+1]+.

Aufarbeitung

  1. additionwas added (5.74 g, 30.8 mmol)
  2. temperaturethe mixture was refluxed for 4.5 hours after which the product
  3. customto precipitate
  4. concentrationThe mixture was concentrated under reduced pressure
  5. customThe product was separated by filtration
  6. washwashed with ethylacetate
  7. customdried at 50° C

Quellen und Nachweise

ORD-Eintrag
ord-183f7a13eb6341c1a117023f1fbe0cec
Quelldatensatz
uspto-grants-2014_11
Patentnummer
US08883791B2

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