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Water → 1H-Pyrazole-1-carboxylic acid, 4,5-dihydro-5-phenyl-, ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl chloroformate | HCID 10928 | — |
| 反応物 | 5-Phenyl-4,5-dihydro-1H-pyrazole | HCID 120841 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 1H-Pyrazole-1-carboxylic acid, 4,5-dihydro-5-phenyl-, ethyl ester | HCID 3079077 | 62% |
反応手順
Triethylamine (2.1 g) was added to a solution of 2.92 g 5-phenyl-2-pyrazoline in 50 ml chloroform, and the mixture was stirred with ice cooling. To the resulting solution, was added dropwise 2.17 g ethyl chloroformate, and the mixture was stirred for one hour. After addition of 50 ml water, the mixture was extracted with 50 ml chloroform, the extract was dried, the dried solution was concentrated, and the residue was purified by silica gel chromatography (chloroform/methanol=100/1), giving 2.7 g (yield: 62%) of pure product as oil. NMR (DMSO-d6): 1.21 (3H, t, J=6 Hz), 2.6-3.7 (2H, m), 4.18 (2H, q, J=6 Hz), 5.22 (1H, dd, J=6, 12 Hz), 6.92 (1H, t, J=2 Hz), 7.1-7.5 (5H, m).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04839376 |
| 出典データセット | uspto-grants-1989_06 |
| ORD ID | ord-607f9f1440894c24a34fcae0d2c9e1f8 |
| 出典メモ | uspto-grants-1989_06 |