化工社化工社 化学情報印刷レポート · 研究参考用
HCID 178452121、化合物 → HCID 178452119、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | HCID 178452121 | HCID 178452121 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | N,N-dimethylformamide ethanol | HCID 19794673 | — |
| 生成物 | HCID 178452119 | HCID 178452119 | 73.8% |
反応手順
4-[(4-Nitro-1H-pyrazole-3-carbonyl)-amino]-piperidine-1-carboxylic acid tert-butyl ester (13.05 g) was dissolved in ethanol/DMF (300 ml/75 ml), treated with 10% palladium on carbon (500 mg) then hydrogenated at room temperature and pressure overnight. The catalyst was removed by filtration through Celite and the filtrate evaporated and re-evaporated with toluene. The crude material was purified by flash column chromatography eluting with EtOAc then 2% MeOH/EtOAc then 5% MeOH/EtOAc. Product containing fractions were combined and evaporated to give 8.78 g of 4-[(4-amino-1H-pyrazole-3-carbonyl)-amino]-piperidine-1-carboxylic acid tert-butyl ester as a brown foam. (LC/MS: Rt 1.91, [M+H]+ 310).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07745638B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-6ce96a5154a4438bac2f558f0b1ed6a2 |
| 出典メモ | uspto-grants-2010_06 |