5-Chlorovaleryl chloride → HCID 19048404、化合物

HRID 233077

反応式

HRID 233077 の反応式
[Cl:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6](Cl)=[O:7].[C:9]([O:12][CH:13]([CH2:42][O:43][C:44](=[O:46])[CH3:45])[CH2:14][NH:15][C:16]([C:18]1[C:23]([I:24])=[C:22]([NH2:25])[C:21]([I:26])=[C:20]([C:27]([NH:29][CH2:30][CH:31]([O:37][C:38](=[O:40])[CH3:39])[CH2:32][O:33][C:34](=[O:36])[CH3:35])=[O:28])[C:19]=1[I:41])=[O:17])(=[O:11])[CH3:10]>>[C:9]([O:12][CH:13]([CH2:42][O:43][C:44](=[O:46])[CH3:45])[CH2:14][NH:15][C:16]([C:18]1[C:23]([I:24])=[C:22]([NH:25][C:6](=[O:7])[CH2:5][CH2:4][CH2:3][CH2:2][Cl:1])[C:21]([I:26])=[C:20]([C:27]([NH:29][CH2:30][CH:31]([O:37][C:38](=[O:40])[CH3:39])[CH2:32][O:33][C:34](=[O:36])[CH3:35])=[O:28])[C:19]=1[I:41])=[O:17])(=[O:11])[CH3:10]

参加物

3

反応物 2

HCID 740895-Chlorovaleryl chlorideHCID 98975345-Amino-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzenedicarboxamide Tetraacetate

生成物 1

HCID 19048404HCID 19048404、化合物収率 97%

実験手順

5-Chloropentanoyl chloride (5.1 g, 33 mmol) was added dropwise to a stirred solution of N,N'-bis[2,3-bis(acetyloxy)propyl]-5-amino-2,4,6-triiodo-1,3-benzenedicarboxamide (20.5 g, 23 mmol) in N,N'-dimethylacetamide (75 ml) at 0°-5°. The reaction mixture was stirred at 5° for 1 hour, and then at room temperature for 30 hours. The solvent was removed in vacuo and the residue was dissolved in ethyl acetate (250 ml). The solution was washed with water (2×50 ml), followed by saturated aqueous NaCl (50 ml), and then dried over anhydrous sodium sulfate. Removal of the solvent in vacuo gave N,N'-bis[2,3-bis(acetyloxy)propyl]-5-[(5-chloro-1-oxopentyl)amino]-2,4,6-triiodo-1,3-benzenedicarboxamide as an off-white fluffy solid (22.1 g, yield 97%, purity 98.5%).

後処理

  1. waitat room temperature for 30 hours
  2. customThe solvent was removed in vacuo
  3. dissolutionthe residue was dissolved in ethyl acetate (250 ml)
  4. washThe solution was washed with water (2×50 ml)
  5. dry with materialdried over anhydrous sodium sulfate
  6. customRemoval of the solvent in vacuo

出典と根拠

ORDレコード
ord-98768679ef16458fb72217710ed3cfe2
出典データセット
uspto-grants-1997_01
特許番号
US05591846

関連ノート

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