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Hydrochloric Acid → 5,6-Dimethoxy-2-[5-methoxy-2-(2-pyridinyl)phenylthio]-1H-benzimidazole

HRID 1199462
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1199462
[CH3:1][O:2][C:3]1[C:21]([O:22][CH3:23])=[CH:20][C:6]2[NH:7][C:8]([S:10][C:11]3[CH:16]=[C:15]([O:17][CH3:18])[CH:14]=[CH:13][C:12]=3N)=[N:9][C:5]=2[CH:4]=1.Cl.N([O-])=O.[Na+].[N:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1>O>[CH3:1][O:2][C:3]1[C:21]([O:22][CH3:23])=[CH:20][C:6]2[NH:7][C:8]([S:10][C:11]3[CH:16]=[C:15]([O:17][CH3:18])[CH:14]=[CH:13][C:12]=3[C:30]3[CH:31]=[CH:32][CH:33]=[CH:34][N:29]=3)=[N:9][C:5]=2[CH:4]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 198667012-[-5,6-Dimethoxy-2-1H-benzimidazolylthio]-4-methoxy benzenamineHCID 23668193Sodium Nitrite

Produkt 1

HCID 198666535,6-Dimethoxy-2-[5-methoxy-2-(2-pyridinyl)phenylthio]-1H-benzimidazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962
Water
Lösungsmittel
2×

Versuchsvorschrift

The product of step (b) above (500 mg) was treated with concentrated hydrochloric acid (0.8 ml) and water (0.8 ml) to form a paste. The paste was stirred at 0°-10° and a solution of sodium nitrite (105 mg) in water (0.5 ml) added dropwise. After stirring for 40 minutes the resultant solution was added slowly to pyridine (5 ml) stirred at 80°. The mixture was stirred for a further 40 minutes then concentrated in vacuo. The residue was slurried with 0.880 ammonia and the mixture again concentrated in vacuo. The residue was slurried with water and extracted with ethyl acetate. The ethyl acetate was washed with water and brine, then dried and evaporated to leave a brown gum. Flash chromatography produced the required product as a pale brown solid, MS MW 393 bp 216.

Aufarbeitung

  1. customto form a paste
  2. stirringstirred at 80°
  3. stirringThe mixture was stirred for a further 40 minutes
  4. concentrationthen concentrated in vacuo
  5. concentrationthe mixture again concentrated in vacuo
  6. extractionextracted with ethyl acetate
  7. washThe ethyl acetate was washed with water and brine
  8. customdried
  9. customevaporated
  10. customto leave a brown gum

Quellen und Nachweise

ORD-Eintrag
ord-49e7dcebdfce42b28d01d0b452cb9002
Quelldatensatz
uspto-grants-1990_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04900751

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