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Triethylamine → 3,4-difluoro-2-(2-fluoro-4-iodo-phenylamino)-N-(2-hydroxy-ethoxy)-5-(2-oxo-tetrahydro-pyrimidin-1-ylmethyl)-benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Di(succinimido) carbonate | HCID 676246 | — |
| 反応物 | 5-[(3-amino-propylamino)-methyl]-3,4-difluoro-2-(2-fluoro-4-iodo-phenylamino)-N-(2-hydroxy-ethoxy)-benzamide | HCID 59347991 | — |
| 溶媒 | Acetonitrile tetrahydrofuran | HCID 22177404 | — |
| 生成物 | 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% |
反応手順
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).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07745663B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-187687b8fb3d433684e8cd7fd4d0ba73 |
| 出典メモ | uspto-grants-2010_06 |