Cyanuric chloride → HCID 58101013, Verbindung

HRID 1097755Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1097755
ClC1N=C(Cl)N=C(Cl)N=1.[CH2:10]([O:17][C:18]1[C:23](=[O:24])[N:22]2[CH:25]=[C:26]([CH3:29])[CH:27]=[CH:28][C:21]2=[N:20][C:19]=1[CH:30]=[N:31]O)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C(OCC)(=O)C>CN(C)C=O>[CH2:10]([O:17][C:18]1[C:23](=[O:24])[N:22]2[CH:25]=[C:26]([CH3:29])[CH:27]=[CH:28][C:21]2=[N:20][C:19]=1[C:30]#[N:31])[C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1

Komponenten

5

Edukt 3

HCID 7954Cyanuric chlorideHCID 8857Ethyl AcetateHCID 76655923HCID 76655923, Verbindung

Produkt 1

HCID 58101013HCID 58101013, VerbindungAusbeute 60,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel2×

Versuchsvorschrift

Trichloro-1,3,5-triazine (576 mg, 3.15 mmol) was dissolved in anhydrous N,N-dimethylformamide (DMF) (1 mL) and stirred at room temperature for 30 min. To this solution was added dropwise a solution of the product from Example 11.1 (927 mg, 3 mmol) in DMF (5 mL). The mixture was kept at room temperature for 2 h, then ethyl acetate (50 mL) was added and the organic phase separated and washed with brine, dried (Na2SO4) and concentrated in vacuo. Purification by short flash chromatography afforded the desired compound (530 mg, 60.7%).

Aufarbeitung

  1. waitThe mixture was kept at room temperature for 2 h
  2. customthe organic phase separated
  3. washwashed with brine
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated in vacuo
  6. customPurification by short flash chromatography

Quellen und Nachweise

ORD-Eintrag
ord-65d2d74aa4d34220a48d26e576fbfa01
Quelldatensatz
uspto-grants-2012_03
Patentnummer
US08143268B2

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