Benzoyl Peroxide → HCID 68632004, Verbindung

HRID 1809469Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1809469
[Br:1][C:2]1[C:3]([CH3:13])=[C:4]([CH:9]=[C:10]([F:12])[CH:11]=1)[C:5]([O:7][CH3:8])=[O:6].C1C(=O)N([Br:21])C(=O)C1.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(Cl)(Cl)(Cl)Cl>[Br:1][C:2]1[C:3]([CH2:13][Br:21])=[C:4]([CH:9]=[C:10]([F:12])[CH:11]=1)[C:5]([O:7][CH3:8])=[O:6]

Komponenten

5

Edukt 3

HCID 7187Benzoyl PeroxideHCID 67184N-bromobutanimideHCID 68633230methyl 3-bromo-5-fluoro-2-methylbenzoate

Produkt 1

HCID 68632004HCID 68632004, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 5943Carbon TetrachlorideLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

A suspension of (E4), NBS (1.2 eq.) and benzoyl peroxide (0.1 eq.) in CCl4 (0.28 M) was heated to reflux for 4.5 h. Afterwards, the reaction mixture was cooled down to 0° C. and the solid filtered off. The solid was washed with Et2O and the filtrate was washed sequentially with 1 M Na2S2O3, brine and dried (Na2SO4). Evaporation of the solvent under reduced pressure afforded the title compound that was used without further purification in the next step. 1H NMR (400 MHz, CDCl3, 300 K) δ 7.63 (1H, dd, J=8.6 and 2.8 Hz), 7.52 (1H, dd, J=7.4 and 2.8 Hz), 5.10 (2H, s), 3.97 (3H, s).

Aufarbeitung

  1. temperaturewas heated
  2. temperatureto reflux for 4.5 h
  3. filtrationthe solid filtered off
  4. washThe solid was washed with Et2O
  5. washthe filtrate was washed sequentially with 1 M Na2S2O3, brine
  6. dry with materialdried (Na2SO4)
  7. customEvaporation of the solvent under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-ed7b6d142d744fc8a1e78924a64e69ba
Quelldatensatz
uspto-grants-2013_01
Patentnummer
US08362030B2

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