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

HRID 376734

반응식

HRID 376734 반응식
[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

참가 물질

3

반응물 1

HCID 88797Benzidine sulfate

생성물 1

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

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

반응 조건

온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5d43279c26b04d69a33773e9367040ec
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06022307

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