N-bromobutanimide → HCID 66967418, Verbindung

HRID 532865Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 532865
Br[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([Cl:9])[C:4]=1[O:10][CH3:11].ClC1C=CC(C)=C(OC)C=1.C1C(=O)[N:26](Br)[C:24](=O)C1>C(Cl)(Cl)Cl.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>[Cl:9][C:5]1[C:4]([O:10][CH3:11])=[C:3]([CH2:2][CH2:24][NH2:26])[CH:8]=[CH:7][CH:6]=1

Komponenten

6

Edukt 3

HCID 67184N-bromobutanimideHCID 2928585-Chloro-2-methylanisoleHCID 19390097HCID 19390097, Verbindung

Produkt 1

HCID 66967418HCID 66967418, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 7187Benzoyl PeroxideKatalysatorHCID 6212ChloroformLösungsmittel

Versuchsvorschrift

1-(bromomethyl)-3-chloro-2-methoxybenzene. A mixture of 4-chloro-2-methoxy-1-methylbenzene (26.5 g, 169 mmol), NBS (33.1 g, 186 mmol) and benzoyl peroxide (200 mg, 0.826 mmol) in CHCl3 was heated to reflux for 24 h. The reaction was allowed to cool to RT and then concentrated in vacuo. The residue was stirred with petroleum ether and the resulting suspension was filtered off and the filtrate was concentrated in vacuo to give the title compound (30.9 g) as brown oil, which was used as it is in the next step. UPLC (2 min) rt 1.708 min.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureto reflux for 24 h
  3. concentrationconcentrated in vacuo
  4. filtrationthe resulting suspension was filtered off
  5. concentrationthe filtrate was concentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-487362bdff01419a99488d3e55d263d9
Quelldatensatz
uspto-grants-2014_10
Patentnummer
US08853203B2

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