関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,2-Dimethylpiperazine | HCID 14664186 | — |
| 反応物 | HCID 178489782 | HCID 178489782 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | HCID 178489807 | HCID 178489807 | 47% |
反応手順
2,2-Dimethylpiperazine (343 mg, 3.00 mmol) was added in one portion to 5-chloro-N-[5-[2-(3,5-dimethoxyphenyl)ethyl]-2H-pyrazol-3-yl]pyrazine-2-carboxamide (388 mg, 1 mmol) in anhydrous dimethylsulfoxide (1.00 ml) at 25° C. The resulting solution was stirred at 100° C. for 18 h. The crude product was purified by ion exchange chromatography, using a SCX column. The desired product was eluted from the column using 7M NH3/MeOH to afford impure material. The concentrated eluent was purified by preparative HPLC, using decreasingly polar mixtures of water (containing 1% NH3) and MeCN as eluents. Fractions containing the desired compound were evaporated to dryness to afford the title compound (217 mg, 47%) as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07737149B2 |
|---|
| 出典データセット | uspto-grants-2010_06 |
|---|
| ORD ID | ord-651a8473ebb444a7b5d7344ddc8de462 |
|---|
| 出典メモ | uspto-grants-2010_06 |
|---|