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Dimethylformamide → 7-Benzyloxy-5-methylthiopyrazolo[1,5-a]pyrimidine-6-carbonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Benzyl Bromide | HCID 7498 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | HCID 178503357 | HCID 178503357 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 7-Benzyloxy-5-methylthiopyrazolo[1,5-a]pyrimidine-6-carbonitrile | HCID 22048079 | 85.2% |
反応手順
80 mg of sodium hydride (60%) was added to 400 mg of 7-hydroxy-5-methylthiopyrazolo[1,5-a]pyrimidine-6-carbonitrile and 6 ml of DMF, followed by stirring at room temperature for about 10 minutes, and then 350 mg of benzyl bromide was added thereto, followed by stirring at about 50° C. overnight. After completion of the reaction, the reaction mixture was cooled to room temperature, about 50 ml of water was added thereto, and the precipitated crystals were collected by filtration, washed with water and dried to obtain crude crystals. The crude crystals were purified by silica gel column chromatography to obtain 490 mg of 7-benzyloxy-5-methylthiopyrazolo[1,5-a]pyrimidine-6-carbonitrile (compound No. 51) having a melting point of 194° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07067520B2 |
| 出典データセット | uspto-grants-2006_06 |
| ORD ID | ord-08952e88222049258a9d087496e1636e |
| 出典メモ | uspto-grants-2006_06 |