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Sulfuric Acid → HCID 20309659、化合物

HRID 437370
ノート
印刷プレビュー

反応式

HRID 437370 の反応式
[NH2:1][C:2]1[C:3]([I:18])=[C:4]([C:8]([I:17])=[C:9]([N:12]([CH3:16])[C:13](=[O:15])[CH3:14])[C:10]=1[I:11])[C:5]([OH:7])=[O:6].[C:19]1(=[O:26])[O:25][C:23](=[O:24])[CH2:22][CH2:21][CH2:20]1.S(=O)(=O)(O)O>O>[C:5]([C:4]1[C:3]([I:18])=[C:2]([C:10]([I:11])=[C:9]([N:12]([CH3:16])[C:13](=[O:15])[CH3:14])[C:8]=1[I:17])[NH:1][C:19](=[O:26])[CH2:20][CH2:21][CH2:22][C:23]([OH:25])=[O:24])([OH:7])=[O:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 7940Glutaric anhydrideHCID 203096823-amino-2,4,6-triiodo-5-(N-methylacetamido)benzoic acid

生成物 1

HCID 20309659HCID 20309659、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 58.6 g. of 3-amino-5-(N-methylacetamido)-2,4,6-triiodobenzoic acid, 74 g. of glutaric anhydride and 8 ml. of concentrated sulfuric acid was heated on a steam bath for five hours. The reaction mixture was poured into water and the solid product collected by filtration. The product, consisting of 3-glutarimido-5-(N-methylacetamido)-2,4,6-triiodobenzoic acid (Example 1) was dissolved in excess dilute aqueous sodium hydroxide, and the solution warmed for thirty minutes, then cooled and 3N hydrochloric acid added slowly until precipitation was complete. The solid product was collected and recrystallized first from acetone, then from acetic acid, and finally from water to give 3'-carboxy-5'-(N-methylacetamido)-2',4',6'-triiodoglutaranilic acid, colorless prisms, m.p. 188.8°-196.0° C.

後処理

  1. additionA mixture of 58.6 g
  2. filtrationthe solid product collected by filtration
  3. dissolutionwas dissolved in excess dilute aqueous sodium hydroxide
  4. temperaturethe solution warmed for thirty minutes
  5. temperaturecooled
  6. addition3N hydrochloric acid added slowly until precipitation
  7. customThe solid product was collected
  8. customrecrystallized first from acetone

出典と根拠

ORDレコード
ord-612f26c485a74b3f835bc2a07923a485
出典データセット
uspto-grants-1977_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04031088

反応ノート

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