化工社化工社 化学情報印刷レポート · 研究参考用
Water → HCID 178473464、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sulfadiazine | HCID 5215 | — |
| 反応物 | Ethyl chloroformate | HCID 10928 | — |
| 反応物 | 4-[3-(4-fluorophenyl)-1H-pyrazol-4-yl]-2-pyrimidinamine | HCID 178508385 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | HCID 178473464 | HCID 178473464 | — |
反応手順
To a suspension of 4-[3-(4-fluorophenyl)-1H-pyrazol-4-yl]-2-pyrimidinamine prepared in accordance with Example A-306 (0.26 g, 0.001 mol) in 5 mL of pyridine was added ethyl chloroformate dropwise. After the addition, the clear solution was stirred at room temperature for 6 hours. Water was added and the aqueous phase was extracted with ethyl acetate. The organic layer was washed with brine, dried over magnesium sulfate and filtered. The filtrate was concentrated and the crude was trituated with ether to give 0.15 g of product, ethyl [4-[3-(4-fluorophenyl)-1H-pyrazol-4-yl]-2-pyrimidinyl]carbamate, as a white solid (46% yield), mp: 163–165° C.; Anal. Calc'd for C16H14FN5O2: C, 58.71; H, 4.31; N, 21.04. Found: C, 59.22; H, 4.51; N, 21.66.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07153959B2 |
| 出典データセット | uspto-grants-2006_12 |
| ORD ID | ord-bce2616eeb604fc2965dac175911b59a |
| 出典メモ | uspto-grants-2006_12 |