4-Chloro-1,2-dinitrobenzene → ethyl P-methyl-2-nitro-5-chlorophenylphosphinate

HRID 463560

Reaktionsgleichung

Reaktionsgleichung von HRID 463560
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[C:4]([N+]([O-])=O)[CH:3]=1.[CH3:14][P:15]([O:19]CC)[O:16][CH2:17][CH3:18]>C(#N)C>[CH3:14][P:15]([C:4]1[CH:3]=[C:2]([Cl:1])[CH:7]=[CH:6][C:5]=1[N+:8]([O-:10])=[O:9])(=[O:19])[O:16][CH2:17][CH3:18]

Komponenten

4

Edukt 2

HCID 330974-Chloro-1,2-dinitrobenzeneHCID 85063Diethyl methylphosphonite

Produkt 1

HCID 53860251ethyl P-methyl-2-nitro-5-chlorophenylphosphinate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

To 4-chloro-1,2-dinitrobenzene (13.2 g, 65.0 mmol) dissolved in acetonitrile (150 ml) is added, dropwise, diethyl methylphosphonite (16.0 g, 117.6 mmol). The mixture is stirred at RT for 20 hours, after which it is concentrated. The crude product is purified by column chromatography (developing with 50% ethyl acetate/hexane) to yield ethyl P-methyl-2-nitro-5-chlorophenylphosphinate.

Aufarbeitung

  1. additionis added
  2. concentrationafter which it is concentrated
  3. customThe crude product is purified by column chromatography (developing with 50% ethyl acetate/hexane)

Quellen und Nachweise

ORD-Eintrag
ord-cd5e6dca7b5048fab9a1583e2647bcfa
Quelldatensatz
uspto-grants-1985_05
Patentnummer
US04520197

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