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二异丙胺 → 5-氰基-2-糠醛
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 二异丙胺 | HCID 7912 | — |
| 反应物 | 2-氰基呋喃 | HCID 69245 | — |
| 反应物 | 磷酸钾 | HCID 516951 | — |
| 反应物 | 正丁基锂 | HCID 178418339 | — |
| 溶剂 | 四氢呋喃 | HCID 8028 | — |
| 溶剂 | 正己烷 | HCID 8058 | — |
| 产物 | 5-氰基-2-糠醛 | HCID 642139 | — |
反应步骤
75 ml of tetrahydrofuran and 22.6 ml of diisopropylamine were cooled to -60° C. and 100 ml of 1.6M n-butyllithium in hexane were added over 25 minutes. The mixture was stirred for 1 hour and 13.02 g of 2-furancarbonitrile in 50 ml of tetrahydrofuran were added. The mixture was stirred for 40 minutes at -70° C. and 13 ml of N-dimethylformamide in 25 ml of tetrahydrofuran were added. The mixture was stirred for 2 hours at -70° C. and then poured into an aqueous potassium dihydrogen phosphate solution and extracted with isopropyl ether. The extract was dried and the solvent was evaporated to obtain after chromatography on silica (eluent: 7/3 hexane/ethyl acetate) 3.51 g of the expected product.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US05405865 |
| 来源数据集 | uspto-grants-1995_04 |
| ORD ID | ord-cd0f69afc8744f378e538c4e26adb6bc |
| 来源说明 | uspto-grants-1995_04 |