Benzidine sulfate → 3,7-Diaminodibenzothiophene-5,5-dioxide

HRID 376734

Reaktionsgleichung

Reaktionsgleichung von HRID 376734
[S:1]([OH:5])(O)(=O)=[O:2].[C:6]1([C:13]2[CH:19]=[CH:18][C:16]([NH2:17])=[CH:15][CH:14]=2)[CH:12]=[CH:11][C:9]([NH2:10])=[CH:8][CH:7]=1>S(=O)(=O)(O)O>[NH2:10][C:9]1[CH:8]=[CH:7][C:6]2[C:13]3[CH:19]=[CH:18][C:16]([NH2:17])=[CH:15][C:14]=3[S:1](=[O:5])(=[O:2])[C:12]=2[CH:11]=1

Komponenten

3

Edukt 1

HCID 88797Benzidine sulfate

Produkt 1

HCID 804123,7-Diaminodibenzothiophene-5,5-dioxideAusbeute 87 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

The title compound was prepared as described in U.S. Pat. Nos. 2,590,632 and 2,620,343. At 10° C., 30 g of benzidine sulfate was added, in portions, to 100 ml of fuming sulfuric acid. After the addition, the reaction was maintained at 70° C. for 18 hours, cooled and poured into 250 g of cracked ice. The beige solid was collected, washed with water and saturated sodium bicarbonate yielding a yellow solid. The yellow solid was stirred with bicarbonate solution 2×, collected, washed with large volumes of water, and dried in vacuo to give 22.66 g (87%) of the desired product.

Aufarbeitung

  1. customThe title compound was prepared
  2. additionAfter the addition
  3. temperaturecooled
  4. customThe beige solid was collected
  5. washwashed with water and saturated sodium bicarbonate yielding a yellow solid
  6. customcollected
  7. washwashed with large volumes of water
  8. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-5d43279c26b04d69a33773e9367040ec
Quelldatensatz
uspto-grants-2000_02
Patentnummer
US06022307

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