Dichloromethane → 2-Nitro-3-Methylbenzotrichloride

HRID 1981684

Reaktionsgleichung

Reaktionsgleichung von HRID 1981684
[N+:1]([C:4]1[C:12]([CH3:13])=[CH:11][CH:10]=[CH:9][C:5]=1[CH:6]([Cl:8])[Cl:7])([O-:3])=[O:2].[N+](C1C(C)=CC=CC=1C[Cl:20])([O-])=O.C(Cl)Cl.[OH-].[Na+]>[Cl-].C([N+](C)(C)C)CCCCCCCCCCC.C(O)(C)(C)C.C(Cl)(Cl)(Cl)Cl>[N+:1]([C:4]1[C:12]([CH3:13])=[CH:11][CH:10]=[CH:9][C:5]=1[C:6]([Cl:20])([Cl:7])[Cl:8])([O-:3])=[O:2]

Komponenten

8

Edukt 4

HCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 13573562HCID 13573562, VerbindungHCID 135735631-(Chloromethyl)-3-methyl-2-nitrobenzene

Produkt 1

HCID 135735652-Nitro-3-Methylbenzotrichloride

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 8152Dodecyltrimethylammonium chlorideKatalysatorHCID 5943Carbon TetrachlorideLösungsmittelHCID 6386tert-ButanolLösungsmittel

Versuchsvorschrift

9.6 gms of 2-nitro-3-methyl benzal chloride (prepared by chlorination of 2-nitro-m-tolualdehyde with thionyl chloride), 9.6 gms of 2-nitro-3-methyl benzyl chloride, 0.6 gms of n-dodecyl trimethyl ammonium chloride, 160 ml of methylene chloride, 100 ml of carbon tetrachloride, 250 ml of 50% sodium hydroxide, and 10 gms of t-butyl alcohol were charged into a reaction vessel. The mixture was refluxed for 31/2 hours, cooled, solvent extracted, distilled and recrystallized to 16.0 gms of product as determined by GC-Mass spectral analysis.

Aufarbeitung

  1. temperatureThe mixture was refluxed for 31/2 hours
  2. temperaturecooled
  3. extractionsolvent extracted
  4. distillationdistilled
  5. customrecrystallized to 16.0 gms of product

Quellen und Nachweise

ORD-Eintrag
ord-90f7aad27e7b4dfdbb6eadc44b9f7309
Quelldatensatz
uspto-grants-1986_06
Patentnummer
US04593144

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