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Sodium Bicarbonate → 2-(2-chlorobenzyl)-3-(2-methanesulfonyl-pyrimidin-4-yl)-6,7-dihydro-5H-pyrazolo[1,2-a]pyrazol-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | Potassium peroxymonosulphate | HCID 10313463 | — |
| 反応物 | Potassium hydroxy sulfite | HCID 23707502 | — |
| 反応物 | 2-(2-chlorobenzyl)-3-(2-methylsulfanyl-pyrimidin-4-yl)-6,7-dihydro-5H-pyrazolo[1,2-a]pyrazol-1-one | HCID 57438071 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | MeOH tetrahydrofuran | HCID 21899815 | — |
| 生成物 | 2-(2-chlorobenzyl)-3-(2-methanesulfonyl-pyrimidin-4-yl)-6,7-dihydro-5H-pyrazolo[1,2-a]pyrazol-1-one | HCID 57438074 | — |
反応手順
To a cold 0° C. solution of 2-(2-chlorobenzyl)-3-(2-methylsulfanyl-pyrimidin-4-yl)-6,7-dihydro-5H-pyrazolo[1,2-a]pyrazol-1-one, 7, (460 mg, 1.23 mmol)) in THF/MeOH (20 mL of 1:1 mixture) is added dropwise a solution of Oxone® (potassium peroxymonosulfate) (3.0 g, 4.9 mmol) in H2O (15 mL). After stirring the reaction for 1.5 hours at room temperature, the solution is poured into aqueous saturated NaHCO3. The aqueous phase is extracted three times with EtOAc and the combined organic layers are washed with brine, dried (MgSO4), filtered, and concentrated in vacuo to afford 316 mg of the desired product which is used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07482356B2 |
| 出典データセット | uspto-grants-2009_01 |
| ORD ID | ord-1f2185a3519e49a3944fd90d5a7c7b7b |
| 出典メモ | uspto-grants-2009_01 |