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HRID 36783作成日:2026年10月25日

Sodium Iodide → HCID 19422762、化合物

https://huagongshe.com/reaction/36783

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium IodideHCID 5238—
反応物Carbonic acid, 1-chloroethyl ethyl esterHCID 162095—
反応物HCID 23692363HCID 23692363—
溶媒DimethylformamideHCID 6228—
生成物HCID 19422762HCID 19422762—

反応条件

温度50 °C

反応手順

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).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05416223
出典データセットuspto-grants-1995_05
ORD IDord-91f97f67ff644647897a849387d38d85
出典メモuspto-grants-1995_05