Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 5-Amino-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzenedicarboxamide Tetraacetate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Acetic Anhydride | HCID 7918 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | 5-Amino-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodoisophthalamide | HCID 10395011 | — |
| 용매 | Pyridine | HCID 1049 | — |
| 생성물 | 5-Amino-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzenedicarboxamide Tetraacetate | HCID 9897534 | — |
반응 단계
5-Amino-2,4,6-triiodo-N,N'-bis(2,3-dihydroxypropyl)-isophthalamide (14.08 g, 0.02 mol), which had been prepared according to GB-A-1548594 was suspended in pyridine (200 ml) and acetic anhydride (57.1 g, 0.56 mol) was added dropwise with stirring and cooling. After stirring overnight, the mixture was poured into ethyl acetate (300 ml) and 20% aqueous HCl (200 ml). After extraction, the organic phase was washed with 2 M aqueous HCl (20 ml), brine (70 ml), dried (Na2SO4) and evaporated. Yield 17.4 g (100%). The crude material was used without further purification, since analysis by HPLC and 1H NMR indicated, that the product was >97% pure.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05958376 |
| 출처 데이터셋 | uspto-grants-1999_09 |
| ORD ID | ord-1ea3159e0afd4efbb1c41f863e2be904 |
| 출처 메모 | uspto-grants-1999_09 |