参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | 海萝胶 | HCID 313 | — |
| 反应物 | N,N-二甲基甲酰胺 | HCID 6228 | — |
| 反应物 | 苯甲腈 | HCID 7505 | — |
| 反应物 | 叠氮化钠 | HCID 33557 | — |
| 催化剂 | 氯化锌 | HCID 3007855 | — |
| 溶剂 | 聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] | HCID 962 | — |
| 产物 | HCID 178418369 | HCID 178418369 | 90.1% |
反应步骤
Zinc chloride (3.3 g, 24.3 mmol, 0.5 eq) was added to 15 mL of N,N-dimethylformamide in small portions while maintaining the temperature below 60° C. The suspension of zinc chloride was cooled to room temperature and treated with 5.0 g of benzonitrile (48.5 mmol, 1.0 eq) followed by 3.2 g of sodium azide (48.5 mmol, 1.0 eq). The heterogeneous mixture was heated at 115° C. with agitation for 18 hours. The mixture was cooled to room temperature, water (30 mL) was added and the mixture acidified by the addition of 5.1 mL of concentrated hydrochloric acid. The mixture was cooled to 0° C. and aged for one hour, then filtered and the filter cake washed with 15 mL of cold 0.1N HCl then dried at 60° C. under vacuum to afford 6.38 g (43.7 mmol, 90%) of the product.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 专利号 | US05726319 |
|---|
| 来源数据集 | uspto-grants-1998_03 |
|---|
| ORD ID | ord-683f6b06ba0444c18452d135760784ee |
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| 来源说明 | uspto-grants-1998_03 |
|---|
