Ammonium Chloride → HCID 14851973, Verbindung

HRID 1032714

Reaktionsgleichung

Reaktionsgleichung von HRID 1032714
[CH3:1][C:2]([CH3:7])([CH3:6])[C:3](Cl)=[O:4].[F:8][C:9]1[CH:14]=[C:13](Cl)[CH:12]=[CH:11][C:10]=1[CH3:16].[Mg].[Cl-].[NH4+:19]>O1CCCC1.N1C=CC=CC=1>[F:8][C:9]1[CH:14]=[C:13]([CH:9]2[CH:14]=[CH:13][N:19]([C:3](=[O:4])[C:2]([CH3:7])([CH3:6])[CH3:1])[CH:11]=[CH:10]2)[CH:12]=[CH:11][C:10]=1[CH3:16]

Komponenten

7

Edukt 4

HCID 25517Ammonium ChlorideHCID 62493Pivaloyl chlorideHCID 5206304-Chloro-2-fluorotolueneHCID 5462224Magnesium

Produkt 1

HCID 14851973HCID 14851973, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1049PyridineLösungsmittelHCID 8028TetrahydrofuranLösungsmittel2×

Reaktionsbedingungen

Temperatur
-40 °C

Versuchsvorschrift

To a solution of 45 ml pyridine in 800 ml tetrahydrofuran (THF) was added dropwise 50 ml trimethylacetyl chloride. The mixture was stirred 3 hrs. at room temperature, 4.0 g cuprous iodide was added, and the mixture stirred for 1 hr. longer. The mixture was then cooled to -40° C. and a Grignard reagent prepared from 45 ml 2-fluoro-4-chlorotoluene and 10 g magnesium in 300 ml THF was added dropwise The reaction mixture was stirred overnight at room temperature, ammonium chloride solution added, and the product was extracted and isolated to give 90 g of an oil used directly in the next reaction.

Aufarbeitung

  1. stirringthe mixture stirred for 1 hr
  2. additionwas added dropwise The reaction mixture
  3. stirringwas stirred overnight at room temperature
  4. extractionthe product was extracted
  5. customisolated

Quellen und Nachweise

ORD-Eintrag
ord-597cc87d81364b66a4448ffc9aee34c3
Quelldatensatz
uspto-grants-1990_09
Patentnummer
US04959363

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