N,N,N',N'-Tetramethylethylenediamine → HCID 19757216, Verbindung

HRID 1588160Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1588160
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH2:10][O:11][CH3:12])[C:6]([O:13][CH3:14])=[CH:5][C:4]=1[O:15][CH2:16][O:17][CH3:18].CN(C)CCN(C)C.[CH2:27]([Li])[CH2:28][CH2:29][CH3:30].ICCCC>C1(C)C=CC=CC=1.CN(C)P(=O)(N(C)C)N(C)C>[CH2:27]([C:8]1[C:7]([O:9][CH2:10][O:11][CH3:12])=[C:6]([O:13][CH3:14])[CH:5]=[C:4]([O:15][CH2:16][O:17][CH3:18])[C:3]=1[O:2][CH3:1])[CH2:28][CH2:29][CH3:30]

Komponenten

7

Edukt 4

HCID 8037N,N,N',N'-TetramethylethylenediamineHCID 10962Butyl iodideHCID 10061046HCID 10061046, VerbindungHCID 178418339Butyllithium

Produkt 1

HCID 19757216HCID 19757216, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1140TolueneLösungsmittelHCID 12679HexamethylphosphoramideLösungsmittel

Versuchsvorschrift

10 Grams of 1,4-dimethoxy-2,5-bis(methoxymethoxy)benzene was dissolved in 200 ml of anhydrous toluene under argon gas stream conditions, to this solution were added 50 ml of hexamethylphosphoric triamide and 8.75 ml of N,N,N',N'-tetramethylethylenediamine (TMEDA), and the mixture was cooled in a dry ice-acetone mixture bath. To this cooled mixture was added dropwise 39 ml of n-butyllithium (1.5 M, n-hexane solution), then stirred the mixture for 30 minutes. Next, 8.9 ml of 1-iodobutane was added to the reaction mixture, and the temperature was back to room temperature by taking for 12 hours. By procedures similar to those described in Reference Example 1, the above-mentioned reaction mixture was purified to obtain 8.5 g of 3-butyl-1,4-dimethoxy-2,5-bis(methoxymethoxy)benzene. Colorless oily substance.

Aufarbeitung

  1. temperaturethe mixture was cooled in a dry ice-acetone mixture bath
  2. customwas back to room temperature
  3. waitby taking for 12 hours
  4. customthe above-mentioned reaction mixture was purified

Quellen und Nachweise

ORD-Eintrag
ord-5b0304f00d6e410b979c27441099d89b
Quelldatensatz
uspto-grants-1993_06
Patentnummer
US05220042

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