Hydrochloric Acid → 1,2,3-Benzothiadiazole-7-carboxylic acid

HRID 1612635

Reaktionsgleichung

Reaktionsgleichung von HRID 1612635
C[O:2][C:3]([C:5]1[C:13]2[S:12][N:11]=[N:10][C:9]=2[CH:8]=[CH:7][CH:6]=1)=[O:4].[OH-].[Na+].O1CCOCC1.Cl>O>[S:12]1[C:13]2[C:5]([C:3]([OH:4])=[O:2])=[CH:6][CH:7]=[CH:8][C:9]=2[N:10]=[N:11]1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 312751,4-DioxaneHCID 1794011,2,3-Benzothiadiazole-7-carboxylic acid, methyl ester

Produkt 1

HCID 109211091,2,3-Benzothiadiazole-7-carboxylic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Reaktionsbedingungen

Temperatur
40 °C

Versuchsvorschrift

100 g (0.51 mol) of 7-methoxycarbonylbenzo-1,2,3-thiadiazole are suspended in 1000 ml of water, and then 310 ml of 2N sodium hydroxide solution and 5 ml of dioxane are added. The reaction mixture is heated to 40° C., is stirred for 4 hours at that temperature and is then cooled to 10° C. A further 1000 ml of water are added and the batch is neutralised with 310 ml of 2N hydrochloric acid. The resulting precipitate is isolated by filtration, lightly dried in a current of air and then dissolved in tetrahydrofuran and the solution is dried over magnesium sulfate, filtered and concentrated. The crystals are suspended in hexane, isolated by filtration and dried.

Aufarbeitung

  1. temperatureis then cooled to 10° C
  2. customThe resulting precipitate is isolated by filtration
  3. customlightly dried in a current of air
  4. dissolutiondissolved in tetrahydrofuran
  5. dry with materialthe solution is dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customisolated by filtration
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-5b24337a92d343fbbef2a65fcdae2f8d
Quelldatensatz
uspto-grants-1993_03
Patentnummer
US05190928

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