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

HRID 376734

反応式

HRID 376734 の反応式
[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

参加物

3

反応物 1

HCID 88797Benzidine sulfate

生成物 1

HCID 804123,7-Diaminodibenzothiophene-5,5-dioxide収率 87%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

反応条件

温度
70 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5d43279c26b04d69a33773e9367040ec
出典データセット
uspto-grants-2000_02
特許番号
US06022307

関連ノート

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