참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Iodide | HCID 5238 | — |
| 반응물 | Carbonic acid, 1-chloroethyl ethyl ester | HCID 162095 | — |
| 반응물 | HCID 23692363 | HCID 23692363 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 19422762 | HCID 19422762 | — |
반응 단계
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).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05416223 |
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| 출처 데이터셋 | uspto-grants-1995_05 |
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| ORD ID | ord-91f97f67ff644647897a849387d38d85 |
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| 출처 메모 | uspto-grants-1995_05 |
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