化工社化工社 化学情報印刷レポート · 研究参考用
Dabco → Ethyl 5-cyclopropylisoxazole-3-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dabco | HCID 9237 | — |
| 反応物 | Ethyl nitroacetate | HCID 69379 | — |
| 反応物 | Cyclopropylacetylene | HCID 138823 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl 5-cyclopropylisoxazole-3-carboxylate | HCID 55251041 | 92.2% |
反応手順
A solution of ethynylcyclopropane (0.40 mL; 4.58 mmol), ethyl 2-nitroacetate (1.30 mL; 11.46 mmol), and 1,4-diazobicyclo[2.2.2]octane (DABCO, 0.053 g; 0.458 mmol) in ethanol (3 mL) was irradiated in a microwave oven at 150° C. for 20 min and was then evaporated. The residue was dissolved in ethyl acetate and the solution was washed with water. The organic layer was evaporated and the residue was purified by flash chromatography on silica gel (eluent: 20 to 100% of dichloromethane in heptane) to afford 0.765 g (92%) of ethyl 5-cyclopropylisoxazole-3-carboxylate as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09434722B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-9e524bd03fb64855931146cbd86ab99c |
| 出典メモ | uspto-grants-2016_09 |