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三乙胺 → HCID 21306993,化合物
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 三乙胺 | HCID 8471 | — |
| 反应物 | 2-(BOC-氨基)-4-羟甲基吡啶 | HCID 23151001 | — |
| 溶剂 | 二甲基亚砜 | HCID 679 | — |
| 产物 | HCID 21306993 | HCID 21306993 | 83% |
反应步骤
(4-Hydroxymethyl-pyridin-2-yl)-carbamic acid tert-butyl ester (1.91 g, 8.51 mmol) was dissolved in dry DMSO (10 mL) and the reaction flask immersed in a waterbath at 15° C. Triethylamine (1.72 g, 17.0 mmol) was added followed by sulfur trioxide pyridine complex (2.41 g, 15.1 mmol). The reaction mixture was stirred for 2 h and poured onto crushed ice and the product extracted with CHCl3. The organic extract was washed with water, dried concentrated under reduced pressure. The crude product was purified by flash chromatography (hexane/EtOAc, 80:20) to give (4-Formyl-pyridin-2-yl)-carbamic acid tert-butyl ester (1.57 g, 83%).
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US07423012B2 |
| 来源数据集 | uspto-grants-2008_09 |
| ORD ID | ord-42f7346519a941639e7046248c9023f6 |
| 来源说明 | uspto-grants-2008_09 |