Triethylamine → HCID 21539424, Verbindung

HRID 1076198Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1076198
[NH2:1][C:2]1[S:3][CH:4]=[C:5]([C:9]([CH3:12])([CH3:11])[CH3:10])[C:6]=1[C:7]#[N:8].[CH3:13][N:14]=[C:15]=[O:16].C(N(CC)CC)C>CN(C)C=O>[C:7]([C:6]1[C:5]([C:9]([CH3:12])([CH3:11])[CH3:10])=[CH:4][S:3][C:2]=1[NH:1][C:15]([NH:14][CH3:13])=[O:16])#[N:8]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 12228Methyl IsocyanateHCID 5968662-Amino-4-(1,1-dimethylethyl)-3-thiophenecarbonitrile

Produkt 1

HCID 21539424HCID 21539424, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of 4 g 2-amino-3-cyano-4-t-butylthiophene, 1.27 g methyl isocyanate and 3 ml triethylamine in 20 ml dimethylformamide was heated at 130°C. for 3 hours and then allowed to stand at about 25°C. overnight. The dimethylformamide was removed by distillation and the residue was crystallized from ether to give the product, as a tan solid, m.p. 212°-214°C. The infrared spectrum of the product showed cyano absorption at 4.6 microns. Sulfur analysis for the product is tabulated in Table I.

Aufarbeitung

  1. customThe dimethylformamide was removed by distillation
  2. customthe residue was crystallized from ether
  3. customto give the product
  4. customcyano absorption at 4.6 microns

Quellen und Nachweise

ORD-Eintrag
ord-29fe9d9ff3f94f46a5d89010d05c1bce
Quelldatensatz
uspto-grants-1976_05
Patentnummer
US03956315

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