Methanol → HCID 44608071, Verbindung

HRID 1943672Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1943672
[Cl:1][C:2]1[C:11]2[N:10]([C:12]([C:14]3[CH:19]=[C:18]([Br:20])[C:17]([O:21]C)=[C:16]([Br:23])[CH:15]=3)=[O:13])[CH2:9][CH2:8][O:7][C:6]=2[CH:5]=[CH:4][N:3]=1.B(Br)(Br)Br.ClCCl.CO>ClC(Cl)C.C(Cl)(Cl)Cl>[Cl:1][C:2]1[C:11]2[N:10]([C:12]([C:14]3[CH:15]=[C:16]([Br:23])[C:17]([OH:21])=[C:18]([Br:20])[CH:19]=3)=[O:13])[CH2:9][CH2:8][O:7][C:6]=2[CH:5]=[CH:4][N:3]=1

Komponenten

7

Edukt 4

HCID 887MethanolHCID 6344DichloromethaneHCID 25134Boron tribromideHCID 86650559HCID 86650559, Verbindung

Produkt 1

HCID 44608071HCID 44608071, VerbindungAusbeute 54 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6212ChloroformLösungsmittelHCID 63651,1-DichloroethaneLösungsmittel

Versuchsvorschrift

In a 5 ml flask equipped with a reflux apparatus, (5-chloro-2,3-dihydro -pyrido[4,3-b][1,4]oxazin-4-yl)-(3,5-dibromo-4-methoxy-phenyl)-methanone (48 mg, 0.1 mmol) was dissolved in dichloroethane (0.5 ml) and chloroform (0.5 ml). 1.0M Boron tribromide dissolved in dichloromethane (1 ml, 1 mmol) was added thereto dropwise at room temperature. The reaction mixture was stirred at 450 for 18 hours. After cooling to room temperature, methanol (1 ml) was added and then stirred at room temperature for 10 minutes. After evaporating under reduced pressure, dichloromethane was added and then stirred. The reaction mixture was filtered to obtain the target compound 30 as white solid (24 mg, 54%).

Aufarbeitung

  1. additionwas added
  2. customdropwise at room temperature
  3. stirringstirred at room temperature for 10 minutes
  4. customAfter evaporating under reduced pressure, dichloromethane
  5. additionwas added
  6. stirringstirred
  7. filtrationThe reaction mixture was filtered

Quellen und Nachweise

ORD-Eintrag
ord-77a1dfff7d904ed8bca5f42ada668eb0
Quelldatensatz
uspto-grants-2013_03
Patentnummer
US08394792B2

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