참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Iodide | HCID 5238 | — |
| 반응물 | Carbonic acid, 1-chloroethyl ethyl ester | HCID 162095 | — |
| 반응물 | Potassium 3,5-diacetylamino-2,4,6-triiodobenzoate | HCID 23692364 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 1-(Ethyloxycarbonyloxy)ethyl 3,5-di(acetylamino)-2,4,6-triiodobenzenecarboxylate | HCID 19422757 | — |
반응 단계
1-Chloroethyl ethyl carbonate (1.68 g, 11.0 mmol) was added at room temperature to a solution of potassium 3,5-di (acetylamino)-2,4,6-triiodobenzenecarboxylate (6.52 g, 10.0 mmol) and sodium iodide (0.30 g, 2.0 mmol) in dry DMF (100 ml). After stirring at 60° C. for 2 hours and at 40° C. for 65 hours the solvent was removed at reduced pressure. The residue was suspended in chloroform (100 and washed four times with a saturated sodium hydrogen carbonate solution and finally twice with water. After drying with magnesium sulfate the solution was evaporated to dryness. Yield: 2.45 g Purity by HPLC: 98.5% 1H-NMR(DMSO-d6): delta=1.24(CH2CH3); 1.63(CHCH3); 2.02(COCH3); 4.20(CH2CH3); 6.93(CHCH3); 10.03 ppm (NH). FAB/MS: 731 (M+H+)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05416223 |
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| 출처 데이터셋 | uspto-grants-1995_05 |
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| ORD ID | ord-6c14c0e043aa46cda61f2d7b2dbbd50d |
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| 출처 메모 | uspto-grants-1995_05 |
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