Sulfuric Acid → Acenaphtho[1,2-b]quinoxaline-2,5-disulfonic acid

HRID 605038

反応式

HRID 605038 の反応式
[S:1](=[O:5])(=[O:4])([OH:3])O.[CH:6]1[C:15]2[C:16]3[C:25]([C:13]4[C:14]=2[C:9]([CH:10]=[CH:11][CH:12]=4)=[CH:8][CH:7]=1)=[N:24][C:23]1[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=1)[N:17]=3>O>[CH:6]1[C:15]2[C:16]3[C:25]([C:13]4[C:14]=2[C:9]([CH:10]=[C:11]([S:1]([OH:3])(=[O:5])=[O:4])[CH:12]=4)=[CH:8][C:7]=1[S:1]([OH:5])(=[O:4])=[O:3])=[N:24][C:23]1[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=1)[N:17]=3

参加物

4

反応物 2

HCID 1118Sulfuric AcidHCID 136028Acenaphtho[1,2-b]quinoxaline

生成物 1

HCID 22141822Acenaphtho[1,2-b]quinoxaline-2,5-disulfonic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

As represented by the following reaction pathway, after 30% fuming sulfuric acid (2.1-liter) was added to 300 g of acenaphtho[1,2-b]quinoxaline obtained by synthesis example 1 and the mixture was stirred at room temperature for 24 hours, the resultant was heated to 130° C. and stirred for 32 hours for reaction. While keeping the obtained solution at 40° C. to 50° C., 4.5-liter of ion exchange water was added for dilution, and the resultant was further stirred for 3 hours. The precipitate was filtered and recrystallized with sulfuric acid to obtain acenaphtho[1,2-b]quinoxaline-2,5-disulfonic acid as represented by the following formula (c).

後処理

  1. customAs represented by the following reaction pathway
  2. customobtained by synthesis example 1
  3. temperaturethe resultant was heated to 130° C.
  4. stirringstirred for 32 hours for reaction
  5. customat 40° C. to 50° C.
  6. stirringthe resultant was further stirred for 3 hours
  7. filtrationThe precipitate was filtered
  8. customrecrystallized with sulfuric acid

出典と根拠

ORDレコード
ord-3c73686c5a3749298a5e9b8df8cb3d5c
出典データセット
uspto-grants-2011_03
特許番号
US07911569B2

関連ノート

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