Sodium Iodide → HCID 19422762、化合物

HRID 36783

反応式

HRID 36783 の反応式
[C:1](=[O:9])([O:6][CH2:7][CH3:8])[O:2][CH:3](Cl)[CH3:4].[C:10]([NH:13][C:14]1[C:15]([I:29])=[C:16]([C:25]([NH:27][CH3:28])=[O:26])[C:17]([I:24])=[C:18]([C:21]([O-:23])=[O:22])[C:19]=1[I:20])(=[O:12])[CH3:11].[K+].[I-].[Na+]>CN(C=O)C>[C:10]([NH:13][C:14]1[C:15]([I:29])=[C:16]([C:25]([NH:27][CH3:28])=[O:26])[C:17]([I:24])=[C:18]([C:21]([O:23][CH:3]([O:2][C:1]([O:6][CH2:7][CH3:8])=[O:9])[CH3:4])=[O:22])[C:19]=1[I:20])(=[O:12])[CH3:11]

参加物

5

反応物 3

HCID 5238Sodium IodideHCID 162095Carbonic acid, 1-chloroethyl ethyl esterHCID 23692363HCID 23692363、化合物

生成物 1

HCID 19422762HCID 19422762、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

1-Chloroethyl ethyl carbonate (1.67 g, 11.0 mmol) was added dropwise at room temperature to a solution of potassium 5-(N-acetylamino)-3-(N-methylaminocarbonyl)-2,4,6-triiodobenzenecarboxylate (6.52 g, 10.0 mmol) and sodium iodide (150 mg, 1.0 mmol) in dry DMF (50 ml). After stirring at 50° C. for 24 hours the solvent was removed at reduced pressure. The residue was dissolved in chloroform and washed four times with a saturated sodium hydrogen carbonate solution and twice with water. After drying with magnesium sulfate and filtration, the solvent was removed at reduced pressure to give the title compound. Yield: (2.2 g, 38 %). Purity by HPLC: 98%. 1H-NMR (DMSO-d6 ): delta=1.24 (t, J=7 Hz, CH3 ); 1.63 (d, J=6 Hz, CH3); 2.03 (s, CH3CO); 2.75 (d, J=3 Hz, NCH3); 4.21 (q, J=7 Hz, CH2): 6.93 (q, J=6 Hz, CH); 8.4-8.7 (m, NHMe); 10.03 ppm (s, NHAc).

後処理

  1. customwas removed at reduced pressure
  2. dissolutionThe residue was dissolved in chloroform
  3. washwashed four times with a saturated sodium hydrogen carbonate solution
  4. dry with materialAfter drying with magnesium sulfate and filtration
  5. customthe solvent was removed at reduced pressure

出典と根拠

ORDレコード
ord-91f97f67ff644647897a849387d38d85
出典データセット
uspto-grants-1995_05
特許番号
US05416223

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