関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 1H-Pyrazole, 3-methyl-4-nitro- | HCID 79255 | — |
| 反応物 | (2S)-2-Methyloxirane | HCID 146262 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | (S)-1-(5-methyl-4-nitro-1H-pyrazol-1-yl)propan-2-ol | HCID 118023522 | 9% |
反応手順
To a solution of 5-methyl-4-nitro-1H-pyrazole (2.5 g, 19.7 mmol) in acetonitrile (100 mL) was added (S)-2-methyloxirane (1.37 g, 23.6 mmol) and cesium carbonate (19.3 g, 59.1 mmol). The mixture was stirred at 30° C. for 7 days, then cooled to room temperature and filtered. The filtrate was concentrated under reduced pressure, and the residue was purified by Prep-HPLC and then chiral-HPLC to give (S)-1-(5-methyl-4-nitro-1H-pyrazol-1-yl)propan-2-ol (0.33 g) as a yellowish solid. MS (ES+) C7H11N3O3 requires: 185, found: 186 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09334263B2 |
|---|
| 出典データセット | uspto-grants-2016_05 |
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| ORD ID | ord-baaa67abe8c24741b659995bc628d4d5 |
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| 出典メモ | uspto-grants-2016_05 |
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