Acetonitrile → HCID 58055793, Verbindung

HRID 408876Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 408876
CS(O[CH2:6][C:7]1[N:12]=[C:11]([C:13]([O:15][CH3:16])=[O:14])[CH:10]=[CH:9][CH:8]=1)(=O)=O.C1([CH2:21][NH:22][C:23]([NH:25][C:26]2[CH:31]=[CH:30][C:29]([C:32]([N:34]3[CH2:39][CH2:38][NH:37][CH2:36][CH2:35]3)=[O:33])=[CH:28][C:27]=2[F:40])=[O:24])CCC1.[C:41](=O)([O-])[O-].[K+].[K+].[C:47](#N)[CH3:48]>>[CH:21]1([NH:22][C:23](=[O:24])[NH:25][C:26]2[CH:31]=[CH:30][C:29]([C:32]([N:34]3[CH2:35][CH2:36][N:37]([CH2:6][C:7]4[N:12]=[C:11]([C:13]([O:15][CH3:16])=[O:14])[CH:10]=[CH:9][CH:8]=4)[CH2:38][CH2:39]3)=[O:33])=[CH:28][C:27]=2[F:40])[CH2:48][CH2:47][CH2:41]1

Komponenten

5

Edukt 4

HCID 6342AcetonitrileHCID 11430Potassium CarbonateHCID 54451634Methyl 6-((methylsulfonyloxy)methyl)picolinateHCID 66661596HCID 66661596, Verbindung

Produkt 1

HCID 58055793HCID 58055793, Verbindung

Versuchsvorschrift

Methyl 6-((methylsulfonyloxy)methyl)picolinate (300 mg, 1.22 mmol), 1-(cyclo-butylmethyl)-3-(2-fluoro-4-(piperazine-1-carbonyl)phenyl)urea (391 mg, 1.22 mmol) and potassium carbonate (505 mg, 3.66 mmol) were combined and stirred in acetonitrile for 18 hours. The reaction mixture was concentrated at reduced pressure. The resulting residue was taken up in dichloromethane, washed with water, dried over sodium sulfate and concentrated under vacuum to afford the title compound (407 mg).

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated at reduced pressure
  2. washwashed with water
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-241998b514e9442493a198ec4a6ba01a
Quelldatensatz
uspto-grants-2014_06
Patentnummer
US08759352B2

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