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 | [1-(N-phenylmethoxycarbonylcarbamimidoyl)pyrrolidin-3-yl]methyl methanesulfonate | HCID 140379087 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | benzyl N-[3-(azidomethyl)pyrrolidine-1-carboximidoyl]carbamate | HCID 140379089 | 68.2% |
反応手順
0.450 g (1.27 mmole) (3RS)-1-(N-benzyloxycarbonylamidino)-3-mesyloxymethyl pyrrolidine and 0.124 g (1.9 mmole) of sodium azide were dissolved in 10 ml dimethylformamide and heated to 60° C. for four hours followed by stirring at room temperature over night. Water was added and the mixture was extracted twice with toluene/ethyl-acetate 2/1. The combined organic layer was dried (Na2SO4), filtered and evaporated. The crude product was purified by flash chromatography using CH2Cl2 /MeOH 95/5 as eluent to yield 0.262 g (68%) of the product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05602253 |
|---|
| 出典データセット | uspto-grants-1997_02 |
|---|
| ORD ID | ord-afd6f3e1777f4bc1bf0cad5e345274cd |
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| 出典メモ | uspto-grants-1997_02 |
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