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Triethylamine → 6-Methyl-2-Trichloromethyl-4-Pyrimidinyl Diphenylcarbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | N,N-Diphenylcarbamic chloride | HCID 65741 | — |
| 反応物 | HCID 178429333 | HCID 178429333 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 6-Methyl-2-Trichloromethyl-4-Pyrimidinyl Diphenylcarbamate | HCID 13041529 | 88% |
反応手順
To a mixture of 5.7 g (0.025 mole) 4-hydroxy-6-methyl-2-trichloromethylpyrimidine, 2.6 g (0.025 mole) triethylamine, and 100 ml acetonitrile was added 5.8 g (0.025 mole) diphenylcarbamoyl chloride. The reaction mixture was refluxed 4 hours. A precipitate was filtered out and ether was added to the filtrate yielding more precipitate. Rotary evaporation gave 9.3 g residue which was recrystallized from ligroin to give 6.15 g (58% yield) of product. An analytical sample was recrystallized a second time from ligroin and had mp 132°-134° C. The structure was confirmed via infrared and elemental analysis.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04343803 |
| 出典データセット | uspto-grants-1982_08 |
| ORD ID | ord-b8dee56bb0454da1acd88ecf3e6eb576 |
| 出典メモ | uspto-grants-1982_08 |