Triethylamine → HCID 20467443, Verbindung

HRID 1903562Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1903562
[CH2:1]([C:3]1[NH:4][CH:5]=[C:6]([CH3:8])[N:7]=1)[CH3:2].C(N(CC)CC)C.[Cl:16][C:17]1[CH:25]=[CH:24][CH:23]=[C:22]([N+:26]([O-:28])=[O:27])[C:18]=1[C:19](Cl)=[O:20]>O1CCCC1.Cl.C(N(CC)CC)C>[Cl:16][C:17]1[CH:25]=[CH:24][CH:23]=[C:22]([N+:26]([O-:28])=[O:27])[C:18]=1[C:19]([N:4]1[CH:5]=[C:6]([CH3:8])[N:7]=[C:3]1[CH2:1][CH3:2])=[O:20]

Komponenten

6

Edukt 3

HCID 8471TriethylamineHCID 22596843HCID 22596843, VerbindungHCID 178437635HCID 178437635, Verbindung

Produkt 1

HCID 20467443HCID 20467443, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8028TetrahydrofuranLösungsmittel2×HCID 11130Triethylamine hydrochlorideLösungsmittel

Versuchsvorschrift

15.4 g of 2-ethyl-4-methyl-imidazole are dissolved in 100 ml of tetrahydrofuran; 14.6 g of triethylamine are added, and there can then added dropwise, within 30 minutes at reflux temperature, 30.8 g of 2-chloro-6-nitrobenzoyl chloride, dissolved in 50 ml of tetrahydrofuran, in the process of which triethylamine hydrochloride precipitates. After 3 hours of refluxing, the mixture is filtered with suction, and the solvent is removed in the rotary evaporator. Recrystallisation of the residue from 85 ml of toluene yields 27.7 g (67.3% of theory) of the desired product, m.p. 119°-120° C.

Aufarbeitung

  1. additionthere can then added dropwise, within 30 minutes
  2. customprecipitates
  3. temperatureAfter 3 hours of refluxing
  4. filtrationthe mixture is filtered with suction
  5. customthe solvent is removed in the rotary evaporator
  6. customRecrystallisation of the residue from 85 ml of toluene

Quellen und Nachweise

ORD-Eintrag
ord-9a2acad788a645d38dc13b894e906a3e
Quelldatensatz
uspto-grants-1984_03
Patentnummer
US04436892

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