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Triethylamine → HCID 178481869、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 1,3-Di-Boc-2-(trifluoromethylsulfonyl)guanidine | HCID 3694570 | — |
| 反応物 | 1H-Pyrazole, 4,5-diamine-1-methyl-, sulfate (1:1) | HCID 21904571 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178481869 | HCID 178481869 | 68.9% |
反応手順
To a solution of 1,3-bis(tert-butoxycarbonyl)-2-(trifluoromethylsulfonyl)guanidine (22.3 g) in dichloromethane (100 ml) were added 4,5-diamino-1-methylpyrazole sulfuric acid salt (10 g) and triethylamine (33.2 ml) at 4° C., and the mixture was stirred at room temperature overnight. The reaction mixture was poured into a mixture of ethyl acetate and water. The aqueous layer was separated, and the organic layer was washed with brine, dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated in vacuo. The concentrate was poured into acetonitrile, and the resulting precipitate was collected by filtration and dried in vacuo to give 5-amino-4-[2′,3′-bis(tert-butoxycarbonyl)guanidino]-1-methylpyrazole (11.62 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07129232B2 |
| 出典データセット | uspto-grants-2006_10 |
| ORD ID | ord-2712a3eda6524cefae95afae20296eb2 |
| 出典メモ | uspto-grants-2006_10 |