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Sulfuric Acid → HCID 20309659、化合物

HRID 1763276
ノート
印刷プレビュー

反応式

HRID 1763276 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 5 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-1e70d7ca24324e55aab40c793997db4e
出典データセット
uspto-grants-1978_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04111937

反応ノート

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