Pyridine → HCID 66635554, Verbindung

HRID 510069Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 510069
[CH3:1][O:2][C:3]1[CH:35]=[C:34]([O:36][CH3:37])[CH:33]=[CH:32][C:4]=1[CH2:5][NH:6][C:7]1[C:12]([NH2:13])=[CH:11][N:10]=[C:9]([C:14]2[C:22]3[C:17](=[N:18][CH:19]=[C:20]([F:23])[CH:21]=3)[N:16]([CH2:24][C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=3[F:31])[N:15]=2)[N:8]=1.[S:38](N)(N)(=[O:40])=[O:39].N1C=CC=CC=1>ClCCl>[CH3:1][O:2][C:3]1[CH:35]=[C:34]([O:36][CH3:37])[CH:33]=[CH:32][C:4]=1[CH2:5][N:6]1[C:7]2[N:8]=[C:9]([C:14]3[C:22]4[C:17](=[N:18][CH:19]=[C:20]([F:23])[CH:21]=4)[N:16]([CH2:24][C:25]4[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=4[F:31])[N:15]=3)[N:10]=[CH:11][C:12]=2[NH:13][S:38]1(=[O:40])=[O:39]

Komponenten

5

Edukt 3

HCID 1049PyridineHCID 82267SulfamideHCID 66614166HCID 66614166, Verbindung

Produkt 1

HCID 66635554HCID 66635554, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
160 °C

Versuchsvorschrift

550 mg (1.093 mmol) of the compound from example 92A were divided between 11 microwave vessels. 50 mg of the substance in each were admixed with 48 mg (0.496 mmol) of sulfamide and 2.5 ml of pyridine and then heated at 160° C. under microwave radiation for 30 min. Subsequently, all batches were combined and freed of the solvent under reduced pressure. The residue was taken up in dichloromethane and extracted three times with water. The phases were separated and the organic phase was dried with sodium sulfate, filtered and concentrated under reduced pressure. The residue was then purified by means of preparative HPLC (acetonitrile:water (+0.05% formic acid) gradient). This gave 0.130 g (12% of theory, purity 50%) of the title compound.

Aufarbeitung

  1. extractionextracted three times with water
  2. customThe phases were separated
  3. dry with materialthe organic phase was dried with sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was then purified by means of preparative HPLC (acetonitrile:water (+0.05% formic acid) gradient)

Quellen und Nachweise

ORD-Eintrag
ord-0bf5ac7f67f44938a149355ffc6439a6
Quelldatensatz
uspto-grants-2015_08
Patentnummer
US09096592B2

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