Methane → 2-[4-(4-Trifluoromethylbenzyloxy)-2-picolylmercapto]-1H-thieno[3,4-d]imidazole

HRID 1196625Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1196625
Cl.Cl.[F:3][C:4]([F:30])([F:29])[C:5]1[CH:28]=[CH:27][C:8]([CH2:9][O:10][C:11]2[CH:16]=[CH:15][N:14]=[C:13]([CH2:17][S:18][C:19]3[NH:23][C:22]4=[CH:24][S:25][CH:26]=[C:21]4[N:20]=3)[CH:12]=2)=[CH:7][CH:6]=1.C(N(CC)CC)C.C>CO>[F:30][C:4]([F:3])([F:29])[C:5]1[CH:28]=[CH:27][C:8]([CH2:9][O:10][C:11]2[CH:16]=[CH:15][N:14]=[C:13]([CH2:17][S:18][C:19]3[NH:23][C:22]4=[CH:24][S:25][CH:26]=[C:21]4[N:20]=3)[CH:12]=2)=[CH:7][CH:6]=1

Komponenten

5

Edukt 3

HCID 297MethaneHCID 8471TriethylamineHCID 198989772-[4-(4-Trifluoromethylbenzyloxy)-2-picolylmercapto]-1H-thieno[3,4-d]imidazole dihydrochloride

Produkt 1

HCID 144259992-[4-(4-Trifluoromethylbenzyloxy)-2-picolylmercapto]-1H-thieno[3,4-d]imidazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

1.5 g (3.0 mmol) of the dihydrochloride from Example 5 are suspended in 25 ml of methanol with ice-cooling and under a nitrogen atmosphere and 1.7 ml (about 12 mmol) of triethylamine are added dropwise, by means of which a clear solution is formed which is subsequently clarified over activated charcoal and concentrated. On treating with water, the residue crystallizes and is washed with water and dried in vacuo, m.p. 141°-143° C. with decomposition.

Aufarbeitung

  1. temperaturecooling and under a nitrogen atmosphere
  2. customis formed which
  3. concentrationconcentrated
  4. additionOn treating with water
  5. customthe residue crystallizes
  6. washis washed with water
  7. customdried in vacuo, m.p. 141°-143° C. with decomposition

Quellen und Nachweise

ORD-Eintrag
ord-4cf7b20f667542b8a11deb620439097e
Quelldatensatz
uspto-grants-1992_05
Patentnummer
US05114955

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