関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Iodopentane | HCID 12335 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Bis(2-pyridylmethyl)amine | HCID 73759 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N,N-bis(pyridin-2-ylmethyl)pentan-1-amine | HCID 58794716 | 72.8% |
反応手順
To 15 ml of N,N-dimethylformamide, 0.85 g potassium hydroxide, 1.0 g di(2-picolyl)amine, and 0.99 g 1-iodopentane were successively added. The mixture was stirred under nitrogen at 35 C for 2.5 hours before an additional 0.99 g 1-iodopentane were added. The mixture was then stirred for 16 hrs at 35 C under nitrogen. The reaction was quenched with 90 ml of water and extracted with two 50 ml portions of ethyl acetate. The combined organic layers were washed with two 25 ml portions of water, dried over anhydrous magnesium sulfate, and filtered. Following solvent removal, the orange oil obtained was purified by silica gel chromatography using a methanol/ethyl acetate mixed solvent system that was ramped from 0% to 10% methanol by volume during the course of the elution. An orange oil (0.98 g) was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08182718B2 |
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| 出典データセット | uspto-grants-2012_05 |
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| ORD ID | ord-4ddc1cc6fcb04b71b859aad11dd6aebc |
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| 出典メモ | uspto-grants-2012_05 |
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