Hydrochloric Acid → 4-Chloro-7-methyl-1,2,3-triazino[4',5'-4,5]thiopheno[2,3-b]pyridine

HRID 1732918Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1732918
[NH2:1][C:2]1[C:10]2[C:5](=[N:6][C:7]([CH3:11])=[CH:8][CH:9]=2)[S:4][C:3]=1[C:12]#[N:13].[ClH:14].[N:15]([O-])=O.[Na+]>O>[Cl:14][C:12]1[C:3]2[S:4][C:5]3[N:6]=[C:7]([CH3:11])[CH:8]=[CH:9][C:10]=3[C:2]=2[N:1]=[N:15][N:13]=1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 7023133-Amino-6-methylthieno[2,3-b]pyridine-2-carbonitrileHCID 23668193Sodium Nitrite

Produkt 1

HCID 4607114-Chloro-7-methyl-1,2,3-triazino[4',5'-4,5]thiopheno[2,3-b]pyridine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To a cold solution of 4.2 g. (0.022 M) of 3-amino-2-cyano-6-methylthieno[2,3-b]pyridine in 30 ml. conc. HCl and 30 ml. HOAC was added a solution of 1.9 g. (0.028 M) of NaNO2 in 20 ml. of H2O. After completion of addition, the ice bath was removed and stirring continued for 2 more hours. The mixture was then poured on ice water and filtered. The crude product was recrystallized from methanol, m.p. 188°-189° C.

Aufarbeitung

  1. additionHOAC was added a solution of 1.9 g
  2. additionAfter completion of addition
  3. customthe ice bath was removed
  4. additionThe mixture was then poured on ice water
  5. filtrationfiltered
  6. customThe crude product was recrystallized from methanol, m.p. 188°-189° C.

Quellen und Nachweise

ORD-Eintrag
ord-c7dec922fb38482a83ffab16ba59e992
Quelldatensatz
uspto-grants-1980_12
Patentnummer
US04239887

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