Boron tribromide → HCID 21706255, Verbindung

HRID 1594922Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1594922
B(Br)(Br)Br.[CH3:5][C:6]1([CH:14]2[NH:20][C:19](=[O:21])[CH2:18][CH2:17][CH2:16][CH2:15]2)[CH:11]=[CH:10][CH:9]=[C:8]([O:12]C)[CH2:7]1>C(Cl)(Cl)Cl>[CH3:5][C:6]1([CH:14]2[NH:20][C:19](=[O:21])[CH2:18][CH2:17][CH2:16][CH2:15]2)[CH:11]=[CH:10][CH:9]=[C:8]([OH:12])[CH2:7]1

Komponenten

4

Edukt 2

HCID 25134Boron tribromideHCID 21706269HCID 21706269, Verbindung

Produkt 1

HCID 21706255HCID 21706255, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

BBr3 (1M in CH2Cl2) (1 mL, 1 mmol) was added dropwise to a solution of 7-(1-methyl-3-methoxyphenyl)-azepan-2-one, as described in Step D above, (0.06 g, 0.26 mmol) in CHCl3 (1 mL) at 0° C. with stirring. The ice bath was removed and stirring was continued for 1 h. The reaction mixture was partitioned between EtOAc (100 mL)—H2O (100 mL), the organic layer separated, washed with H2O, dried (MgSO4), filtered and concentrated to give the title compound after SiO2 chromatography (CHCl3:MeOH, 10:1).

Aufarbeitung

  1. customat 0° C.
  2. customThe ice bath was removed
  3. stirringstirring
  4. customThe reaction mixture was partitioned between EtOAc (100 mL)—H2O (100 mL)
  5. customthe organic layer separated
  6. washwashed with H2O
  7. dry with materialdried (MgSO4)
  8. filtrationfiltered
  9. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-ba9941c0c4ea4de9add891c79c61b6a5
Quelldatensatz
uspto-grants-2001_09
Patentnummer
US06284755B1

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