反応式
Cl[CH:2]1[CH2:6][O:5][C:4](=[O:7])[O:3]1.[C:8]([NH:11][C:12]1[C:13]([I:28])=[C:14]([N:23]([C:25](=[O:27])[CH3:26])[CH3:24])[C:15]([I:22])=[C:16]([C:19]([O-:21])=[O:20])[C:17]=1[I:18])(=[O:10])[CH3:9].[K+].[I-].[Na+]>CN(C=O)C>[O:5]1[CH2:6][CH:2]([O:21][C:19]([C:16]2[C:17]([I:18])=[C:12]([NH:11][C:8](=[O:10])[CH3:9])[C:13]([I:28])=[C:14]([N:23]([C:25](=[O:27])[CH3:26])[CH3:24])[C:15]=2[I:22])=[O:20])[O:3][C:4]1=[O:7]参加物
反応物 3
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 50 °C
実験手順
4-Chloro-1,3-dioxolan-2-one (1.35 g, 11 mmol) was added at room temperature to a solution of potassium 5-(N-acetylamino)-3-(N-acetyl-N-methylamino)-2,4,6-triiodobenzenecarboxylate (6.66 g, 10 mmol) and sodium iodide (0.15 g, 1 mmol) in dry DMF (50 ml). After stirring at 50° C. for 6 hours and at room temperature for 4 days the solvent was removed at reduced pressure. The residue was dissolved in chloroform (100 ml) and washed four times with a saturated sodium hydrogen carbonate solution and finally twice with water. After treatment with magnesium sulfate the solution was finally evaporated to dryness. Yield: 5.6 g. Purity by HPLC: 93%. 1H-NMR (DMSO-d6): delta=1.67 (N(CH3)COCH3); 2.05(NCOCH3); 2.96(NCH3); 4.7; 4.9(CH2); 7.02(CH); 10.14 ppm(NH).
後処理
- customwas removed at reduced pressure
- dissolutionThe residue was dissolved in chloroform (100 ml)
- washwashed four times with a saturated sodium hydrogen carbonate solution
- customAfter treatment with magnesium sulfate the solution was finally evaporated to dryness
出典と根拠
- ORDレコード
- ord-274ce378302f483fbc524d45a183068a
- 出典データセット
- uspto-grants-1995_05
- 特許番号
- US05416223
関連ノート
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