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Trityl chloride → Dimethyl 1-trityl-3,5-pyrazoledicarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trityl chloride | HCID 6456 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 3,5-dimethyl 1H-pyrazole-3,5-dicarboxylate | HCID 1484491 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | N,N-Dimethylformamide--water (1/1) | HCID 21962138 | — |
| 生成物 | Dimethyl 1-trityl-3,5-pyrazoledicarboxylate | HCID 12377531 | — |
反応手順
To a solution of 1.84 g. (10 mmol) of 3,5-pyrazoledicarboxylic acid dimethyl ester* in 15 ml. of DMF, stirred at 0° under argon, was added 480 mg. (10 mmol) of 50% NaH (suspension in mineral oil). After the evolution of hydrogen had ceased, 2.7 g. (10 mmol) of triphenylmethyl chloride in 20 ml. of DMF was added dropwise. The mixture was allowed to warm to room temperature, stirred 1.5 hours, poured into H2O, and the resulting precipitate filtered. After recrystallization from 2-ethoxyethanol-H2O, there was obtained the end product. The analytical sample was obtained as colorless needles by recrystallization from DMF-H2O; mp 212°-213.5°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04157331 |
| 出典データセット | uspto-grants-1979_06 |
| ORD ID | ord-33f2f6c2ddd84ba9ae4205c636ff5b3b |
| 出典メモ | uspto-grants-1979_06 |