Hydrochloric Acid → 5-Amino-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzenedicarboxamide Tetraacetate

HRID 618918

反応式

HRID 618918 の反応式
[NH2:1][C:2]1[C:3]([I:26])=[C:4]([C:18]([NH:20][CH2:21][CH:22]([OH:25])[CH2:23][OH:24])=[O:19])[C:5]([I:17])=[C:6]([C:15]=1[I:16])[C:7]([NH:9][CH2:10][CH:11]([OH:14])[CH2:12][OH:13])=[O:8].C(O[C:31](=[O:33])[CH3:32])(=O)C.C([O:37][CH2:38][CH3:39])(=O)C.Cl>N1C=CC=CC=1>[NH2:1][C:2]1[C:15]([I:16])=[C:6]([C:7]([NH:9][CH2:10][CH:11]([O:14][C:31](=[O:33])[CH3:32])[CH2:12][O:13][C:38](=[O:37])[CH3:39])=[O:8])[C:5]([I:17])=[C:4]([C:3]=1[I:26])[C:18]([NH:20][CH2:21][CH:22]([O:25][C:12](=[O:13])[CH3:11])[CH2:23][O:24][C:7](=[O:8])[CH3:6])=[O:19]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 8857Ethyl AcetateHCID 103950115-Amino-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide

生成物 1

HCID 98975345-Amino-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzenedicarboxamide Tetraacetate

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

5-Amino-2,4,6-triiodo-N,N'-bis(2,3-dihydroxypropyl)-isophthalamide (14.08 g, 0.02 mol), which had been prepared according to GB-A-1548594 was suspended in pyridine (200 ml) and acetic anhydride (57.1 g, 0.56 mol) was added dropwise with stirring and cooling. After stirring overnight, the mixture was poured into ethyl acetate (300 ml) and 20% aqueous HCl (200 ml). After extraction, the organic phase was washed with 2 M aqueous HCl (20 ml), brine (70 ml), dried (Na2SO4) and evaporated. Yield 17.4 g (100%). The crude material was used without further purification, since analysis by HPLC and 1H NMR indicated, that the product was >97% pure.

後処理

  1. temperaturecooling
  2. stirringAfter stirring overnight
  3. extractionAfter extraction
  4. washthe organic phase was washed with 2 M aqueous HCl (20 ml), brine (70 ml)
  5. dry with materialdried (Na2SO4)
  6. customevaporated
  7. customThe crude material was used without further purification, since analysis by HPLC and 1H NMR

出典と根拠

ORDレコード
ord-1ea3159e0afd4efbb1c41f863e2be904
出典データセット
uspto-grants-1999_09
特許番号
US05958376

関連ノート

読み込み中…