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Trifluoroacetic acid → HCID 178481638、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | Trifluoromethanesulfonic acid | HCID 62406 | — |
| 反応物 | HCID 178490875 | HCID 178490875 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178481638 | HCID 178481638 | 96% |
反応手順
To a solution of 7-(4-Methoxybenzyl)-5-methyl-3-(phenylamino)-1H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione (6.6 g, 17.5 mmol) in CH2Cl2 (200 mL) is added TFA (30 mL) slowly at room temperature, followed by adding trifluoromethanesulfonic acid (10 mL) dropwise. After the reaction-mixture is stirred at r.t. for 2 hours, solvent is removed under reduced pressure, and then 200 mL of 1N NaOH is added with cooling. The mixture is extracted with ethyl acetate five times, dried over Na2SO4, and then filtered. The filtrate is evaporated to dryness to give 4.3 g of crude product as white solids (Yield: 96%). MS (ESI) m/z 258.1 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08829008B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-a704007e81294b31bd1b4c2c7307d379 |
| 出典メモ | uspto-grants-2014_09 |