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Triethylamine → N'-[2-(2,4,6-Trimethyl-phenyl)-acetyl]-hydrazinecarboxylic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Hydrazinecarboxylic acid, ethyl ester | HCID 20064 | — |
| 反応物 | 2,4,6-Trimethylbenzeneacetyl chloride | HCID 11030754 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N'-[2-(2,4,6-Trimethyl-phenyl)-acetyl]-hydrazinecarboxylic acid ethyl ester | HCID 71145194 | — |
反応手順
To a solution of hydrazinecarboxylic acid ethyl ester (ethyl carbazate, 32.8 g, 314.9 mmol) and triethylamine (44.1 ml, 32.0 g, 316.4 mmol) in tetrahydrofuran (1000 ml) at 0° C. was added (2,4,6-trimethyl-phenyl)-acetyl chloride (62.0 g, 315.2 mmol) dropwise. The thick suspension was stirred at room temperature for one hour and the solvent evaporated. The residue was suspended in a mixture of t-butyl methyl ether (500 ml) and water (500 ml), stirred, filtered and the solid washed with small portions of water and t-butyl methyl ether. The solid was dried in vacuo over phosphorus pentoxide at 40° C. Yield: 78.4 g of N′-[2-(2,4,6-trimethyl-phenyl)-acetyl]-hydrazinecarboxylic acid ethyl ester as a white solid, mp 184-186° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09282743B2 |
| 出典データセット | uspto-grants-2016_03 |
| ORD ID | ord-c27fa7da8c534a81938e2e94d88e8c28 |
| 出典メモ | uspto-grants-2016_03 |