Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 3,4-difluoro-2-(2-fluoro-4-iodo-phenylamino)-N-(2-hydroxy-ethoxy)-5-(2-oxo-tetrahydro-pyrimidin-1-ylmethyl)-benzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Di(succinimido) carbonate | HCID 676246 | — |
| 반응물 | 5-[(3-amino-propylamino)-methyl]-3,4-difluoro-2-(2-fluoro-4-iodo-phenylamino)-N-(2-hydroxy-ethoxy)-benzamide | HCID 59347991 | — |
| 용매 | Acetonitrile tetrahydrofuran | HCID 22177404 | — |
| 생성물 | 3,4-difluoro-2-(2-fluoro-4-iodo-phenylamino)-N-(2-hydroxy-ethoxy)-5-(2-oxo-tetrahydro-pyrimidin-1-ylmethyl)-benzamide | HCID 11570424 | 61.2% |
반응 단계
The amine synthesized in Step A (66.4 mg, 0.1233 mmol) was dissolved in THF:CH3CN (1:1 v/v, 3.0 ml). N,N-disuccinimidyl carbonate (47.4 mg, 1.5 eq., 0.1849 mmol) and triethylamine (103.1 μl, 6.0 eq., 0.7398 mmol) were added sequentially to this solution, and the mixture was stirred at room temperature for 20 hours. The solvent was removed under reduced pressure, and the residue was purified by LC/MS to give white crystals (42.6 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08575391B2 |
| 출처 데이터셋 | uspto-grants-2013_11 |
| ORD ID | ord-cb017b8eb39d4e5ca03e452baacee576 |
| 출처 메모 | uspto-grants-2013_11 |