Triethylamine → HCID 178443160, Verbindung

HRID 903304Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 903304
[CH2:1]([O:15][C:16]1[CH:25]=[CH:24][CH:23]=[CH:22][C:17]=1[C:18](=[O:21])[CH2:19]Br)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].[NH:26]1[CH:30]=[N:29][N:28]=[N:27]1.C(N(CC)CC)C>C(#N)C>[NH:26]1[C:30]([CH2:19][C:18]([C:17]2[CH:22]=[CH:23][CH:24]=[CH:25][C:16]=2[O:15][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14])=[O:21])=[N:29][N:28]=[N:27]1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 20516628HCID 20516628, VerbindungHCID 178418441HCID 178418441, Verbindung

Produkt 1

HCID 178443160HCID 178443160, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel2×

Versuchsvorschrift

To a solution of 14.6 g of o-tetradecyloxyphenacylbromide in 75 ml of acetonitrile was added a solution of 2.8 g of tetrazole and 4.0 g of triethylamine in 75 ml of acetonitrile. The reaction mixture was stirred at reflux temperature for 2 hours then evaporated to dryness. The residue was dissolved in chloroform and the organic layer washed with water, dried over magnesiumsulfate, filtered and evaporated to give the crude compound. Recrystallisation from petrol (b.p. 60°-80° C.) gave the acetophenone derivative as a fine white powder. Yield: 12.7 g; m.p. 67° to 69° C.

Aufarbeitung

  1. temperatureat reflux temperature for 2 hours
  2. customthen evaporated to dryness
  3. dissolutionThe residue was dissolved in chloroform
  4. washthe organic layer washed with water
  5. dry with materialdried over magnesiumsulfate
  6. filtrationfiltered
  7. customevaporated
  8. customto give the crude compound
  9. customRecrystallisation from petrol (b.p. 60°-80° C.)

Quellen und Nachweise

ORD-Eintrag
ord-1c134ee3be2a42ecaedc855b2a855812
Quelldatensatz
uspto-grants-1980_10
Patentnummer
US04226934

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