関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfoxide | HCID 679 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | (5-methyl-1-pyridin-2-yl-1H-pyrazol-4-yl)-methanol | HCID 66438330 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Sodium Bicarbonate | HCID 516892 | — |
| 生成物 | 5-Methyl-1-pyridin-2-yl-1H-pyrazole-4-carbaldehyde | HCID 21097352 | — |
反応手順
Dissolve dimethyl sulfoxide (0.751 mL, 10.6 mmol) in DCM (20 mL) and cool to −78° C. Add oxalyl chloride (0.577 mL, 6.62 mmol) dropwise in DCM (8 mL) and stir for 15 min. Add (5-methyl-1-pyridin-2-yl-1H-pyrazol-4-yl)-methanol (0.501 g, 2.65 mmol) in DCM (20 mL) dropwise and stir for one hr. at −78° C. Add triethylamine (1.85 mL, 13.2 mmol) and warm the mixture to room temperature for one hr. Dilute the mixture with saturated sodium bicarbonate and extract 3 times with DCM. Dry (sodium sulfate) the solution, filter and concentrate to give the title preparation as a white solid (0.496 g, 100%). MS (ES): m/z=188 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08202873B2 |
|---|
| 出典データセット | uspto-grants-2012_06 |
|---|
| ORD ID | ord-ed62302a164a4ba78d7e2b01acc774c4 |
|---|
| 出典メモ | uspto-grants-2012_06 |
|---|
