参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | 聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] | HCID 962 | — |
| 反应物 | 叠氮化钠 | HCID 33557 | — |
| 反应物 | [1-(N-phenylmethoxycarbonylcarbamimidoyl)pyrrolidin-3-yl]methyl methanesulfonate | HCID 140379087 | — |
| 溶剂 | N,N-二甲基甲酰胺 | HCID 6228 | — |
| 产物 | benzyl N-[3-(azidomethyl)pyrrolidine-1-carboximidoyl]carbamate | HCID 140379089 | 68.2% |
反应步骤
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.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 专利号 | US05723444 |
|---|
| 来源数据集 | uspto-grants-1998_03 |
|---|
| ORD ID | ord-8f9821df03a7466091a3423b9a248655 |
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| 来源说明 | uspto-grants-1998_03 |
|---|
