反応式
[C:1](=[O:13])([O:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[O:2][CH:3](Cl)[CH3:4].[C:14]([NH:17][C:18]1[C:19]([I:34])=[C:20]([N:29]([C:31](=[O:33])[CH3:32])[CH3:30])[C:21]([I:28])=[C:22]([C:25]([O-:27])=[O:26])[C:23]=1[I:24])(=[O:16])[CH3:15].[K+].[I-].[K+]>CN(C=O)C>[C:14]([NH:17][C:18]1[C:19]([I:34])=[C:20]([N:29]([C:31](=[O:33])[CH3:32])[CH3:30])[C:21]([I:28])=[C:22]([C:25]([O:27][CH:3]([O:2][C:1]([O:6][C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[O:13])[CH3:4])=[O:26])[C:23]=1[I:24])(=[O:16])[CH3:15]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
1-Chloroethyl phenyl carbonate (prepared according to Synthesis 1986, 627) (2.21 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 potassium iodide (0.17 g, 1 mmol) in dry DMF. 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 suspended in chloroform (100 ml) and washed four times with a saturated sodium hydrogen carbonate solution and twice with water. After drying with magnesium sulfate the solution was evaporated to dryness. Yield: 7.3 g. Purity by HPLC: 98%. 1H-NMR (DMSO-d6): delta=1.68 (N(CH3)COCH3); 1.74 (CHCH3); 2.05 (NCOCH3); 2.97 (NCH3); 7.05 (CH); 7.25-7.52 (arom.); 10.14 ppm (NH).
後処理
- customwas removed at reduced pressure
- washwashed four times with a saturated sodium hydrogen carbonate solution
- dry with materialAfter drying with magnesium sulfate the solution
- customwas evaporated to dryness
出典と根拠
- ORDレコード
- ord-e23a9c7d5cff4733865868ed2fda8809
- 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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