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(3-(Trifluoromethyl)phenyl)hydrazine → 5-Cyclopropyl-3-pyridin-3-yl-1-(3-trifluoromethyl-phenyl)-1H-pyrazole-4-carboxylic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | (3-(Trifluoromethyl)phenyl)hydrazine | HCID 98650 | — |
| 反応物 | 3-Cyclopropyl-3-oxo-2-(pyridine-3-carbonyl)-propionic acid methyl ester | HCID 67314284 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 5-Cyclopropyl-3-pyridin-3-yl-1-(3-trifluoromethyl-phenyl)-1H-pyrazole-4-carboxylic acid methyl ester | HCID 67315175 | 8.5% |
反応手順
A solution of gave 3-cyclopropyl-3-oxo-2-(pyridine-3-carbonyl)-propionic acid methyl ester (326 mg, 1.25 mmol) and 3-(trifluoromethyl)phenylhydrazine (220 mg, 1.12 mmol) in 2 ml acetic acid was stirred 20 h at room temperature. The reaction mixture was evaporated, the residue treated with EtOAc:n-heptane 1:1 and filtered off. The filtrate was concentrated in vacuo and chromatographed (amino-phase silica gel, EtOAc:n-heptane 1:1) to yield the title compound as a light yellow gum (37 mg, 8%). MS: 388.3 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07977358B2 |
| 出典データセット | uspto-grants-2011_07 |
| ORD ID | ord-23564c8463d0468fbed8058fd5aa9cf9 |
| 出典メモ | uspto-grants-2011_07 |