1,2-Dichlorobenzene → HCID 19021367, Verbindung

HRID 1108948Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1108948
[CH3:1][N:2](S(C1C=CC=CC=1)(=O)=O)[N:3]=[C:4](Cl)[C:5]1[C:10]([Cl:11])=[CH:9][CH:8]=[CH:7][C:6]=1[Cl:12].[CH2:23]([O:33][C:34]1[CH:41]=[CH:40][C:37]([C:38]#[N:39])=[CH:36][CH:35]=1)[CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32].[Cl-].[Al+3].[Cl-].[Cl-].ClC1C=CC=CC=1Cl>C(Cl)(Cl)Cl>[CH2:23]([O:33][C:34]1[CH:41]=[CH:40][C:37]([C:38]2[N:2]([CH3:1])[N:3]=[C:4]([C:5]3[C:6]([Cl:12])=[CH:7][CH:8]=[CH:9][C:10]=3[Cl:11])[N:39]=2)=[CH:36][CH:35]=1)[CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32]

Komponenten

6

Edukt 4

HCID 72391,2-DichlorobenzeneHCID 6451240Aluminum(III) ChlorideHCID 190213714-(Decyloxy)benzonitrileHCID 54261612HCID 54261612, Verbindung

Produkt 1

HCID 19021367HCID 19021367, VerbindungAusbeute 32,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Reaktionsbedingungen

Temperatur
140 °C

Versuchsvorschrift

A mixture of 1.10 g of N-methyl-N-phenylsulfonyl-2,6-dichlorobenzohydrazonoyl chloride, 0.70 g of 4-decyloxybenzonitrile, 0.4 g of anhydrous aluminium chloride and 3 ml of o-dichlorobenzene was stirred in an oil bath at a temperature of 140° C. for 30 minutes. After the cooling, the resulting solution was dissolved in 100 ml of chloroform, washed with diluted hydrochloric acid solution, diluted sodium hydroxide solution and saline water in this order, dried over anhydrous magnesium sulfate and concentrated under a reduced pressure. The resulting concentrate was purified through a chromatography of silica gel column using a mixed solution of hexane and ethyl acetate as a developing solvent to obtain 0.40 g of the given compound (melting point: 60.0°-64.0° C.).

Aufarbeitung

  1. washwashed with diluted hydrochloric acid solution, diluted sodium hydroxide solution and saline water in this order
  2. dry with materialdried over anhydrous magnesium sulfate
  3. concentrationconcentrated under a reduced pressure
  4. concentrationThe resulting concentrate
  5. customwas purified through a chromatography of silica gel column

Quellen und Nachweise

ORD-Eintrag
ord-b00c3026da4247f0978f845febb022a9
Quelldatensatz
uspto-grants-1994_06
Patentnummer
US05318959

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