N-bromobutanimide → HCID 66967418, Verbindung

HRID 926238Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 926238
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

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-5704c7ec77fe40f696e68774708bafdc
Quelldatensatz
uspto-grants-2016_03
Patentnummer
US09284331B2

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