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p-Toluenesulfonic acid → 1-ethyl 1-(tetrahydro-2H-pyran-2-yloxy)cyclopropanecarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 3,4-dihydro-2H-pyran | HCID 8080 | — |
| 反応物 | Ethyl 1-hydroxycyclopropane-1-carboxylate | HCID 2733706 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-ethyl 1-(tetrahydro-2H-pyran-2-yloxy)cyclopropanecarboxylate | HCID 90010340 | 87.5% |
反応手順
To a solution of ethyl 1-hydroxycyclopropanecarboxylate (1040 mg, 8.000 mmol) and PTSA (137 mg, 0.800 mmol) in DCM (20 mL) was added a solution of DHP (1344 mg, 16.00 mmol) in DCM (10 mL) dropwise at 0° C. The mixture was stirred for 20 h at room temperature. After concentration, the residue was purified by silica gel column chromatography eluting with petroleum ether/ethyl acetate (10/1) to afford the title compound (1500 mg, 85%) as oil. LC-MS (ESI): m/z=215 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09212173B2 |
| 出典データセット | uspto-grants-2015_12 |
| ORD ID | ord-63720363da2249dfab3a43238ad45427 |
| 出典メモ | uspto-grants-2015_12 |