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三氟乙酸乙酯 → Acetamide, N-(2-aminocyclohexyl)-2,2,2-trifluoro-, cis-
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 三氟乙酸乙酯 | HCID 9794 | — |
| 反应物 | 顺式-1,2-环己二胺 | HCID 342917 | — |
| 溶剂 | 乙醇 | HCID 702 | — |
| 产物 | Acetamide, N-(2-aminocyclohexyl)-2,2,2-trifluoro-, cis- | HCID 11042018 | — |
反应步骤
cis-Cyclohexane-1,2-diamine (5.00 g, 43.9 mmol, 1.00 eq) was charged to a 250 mL three-neck round bottom flask equipped with an overhead stirrer and a thermocouple. Ethanol (50 mL) was added and the solution was cooled to <0° C. using an ice-brine bath. A solution of ethyl trifluoroacetate (6.23 g, 1.00 eq) in EtOH (25 mL) was added via a syringe pump over a one hour period. Once the addition was complete, the cooling bath was removed and the solution was slowly warmed to RT and stirred for 3.5 hours to afford the title compound in EtOH. Half (41 mL, about 21.9 mmol) of the total solution (about 82 mL) was carried into the next step.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US09108970B2 |
| 来源数据集 | uspto-grants-2015_08 |
| ORD ID | ord-ad0d059b0c884f9ea153fc014d040e82 |
| 来源说明 | uspto-grants-2015_08 |