関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Azide | HCID 33557 | — |
| 反応物 | 2-[1-(N-phenylmethoxycarbonylcarbamimidoyl)piperidin-4-yl]ethyl methanesulfonate | HCID 140379084 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | benzyl N-[4-(2-azidoethyl)piperidine-1-carboximidoyl]carbamate | HCID 140379074 | — |
反応手順
In 100 ml of dimethylformamide was dissolved 4.4 g (0.0115 mol) of crude 1-benzyloxycarbonylamidino-4-mesyloxyethyl piperidine and 4.5 g (0.069 Mol) of sodium azide was added. The mixture was heated at 100° C. for 2.5 h. It was then poured into water and extracted with ethyl acetate three times. The combined organic phase was washed with water, dried (Na2SO4) and evaporated. The residue was flash chromatographed on silica gel using ethyl acetate/heptane 1/1 as eluent. Yield: 3.0 g (79%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06984627B1 |
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| 出典データセット | uspto-grants-2006_01 |
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| ORD ID | ord-a73614eb32cd4e089303c1e43a2034d0 |
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| 出典メモ | uspto-grants-2006_01 |
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