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Acetonitrile → HCID 22048085、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Pyridinemethanamine | HCID 77317 | — |
| 反応物 | 7-Chloro-5-methylthiopyrazolo[1,5-a]pyrimidine-6-carbonitrile | HCID 22048080 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 22048085 | HCID 22048085 | 77.4% |
反応手順
A mixture comprising 460 mg of 4-picolylamine, 430 mg of triethylamine and 1 ml of acetonitrile was dropwise added to 950 mg of 7-chloro-5-methylthiopyrazolo[1,5-a]pyrimidine-6-carbonitrile and 20 ml of acetonitrile under cooling with ice, followed by stirring for about 1 hour. After completion of the reaction, about 80 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 970 mg of 7-(4-pyridylmethyl)amino-5-methylthiopyrazolo[1,5-a]pyrimidine-6-carbonitrile (compound No. 3) having a melting point of from 153 to 154° 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-063ee40dd54c4fe2815b2952630b9b8a |
| 出典メモ | uspto-grants-2006_06 |