関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Azidotrimethylsilane | HCID 78378 | — |
| 反応物 | 6-fluoro-N-methoxy-N-methylpicolinamide | HCID 59700620 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 6-Azido-pyridine-2-carboxylic acid methoxy-methyl-amide | HCID 57942204 | 25% |
反応手順
A mixture of 6-fluoro-pyridine-2-carboxylic acid methoxy-methyl-amide (1.19 g, 6.47 mmol) and azido-trimethylsilane (2.0 g, 16.8 mmol) in DMF (10 mL) was stirred at 110° C. for 72 h. The reaction mixture was diluted with 50 mL of dichloromethane and washed with water (3×50 mL). The organic layer was separated, evaporated to dryness, and subjected to column chromatography (SiO2, 40% EtOAc-hexanes) to obtain 6-azido-pyridine-2-carboxylic acid methoxy-methyl-amide (0.335 g) in 25% yield. ESMS m/z (relative intensity): 208 (M+H)+ (100).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08093247B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-54e4ba292a5c43fba83ab73e8e8a8708 |
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| 出典メモ | uspto-grants-2012_01 |
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