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Phosgene → N-pentyl-N-phenylcarbamoyl chloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosgene | HCID 6371 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | N-Pentylaniline | HCID 75865 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | N-pentyl-N-phenylcarbamoyl chloride | HCID 18965165 | 98.3% |
反応手順
A solution of 4.05 g (24.8 mmole) of N-Pentylaniline (from Step A) in 45 ml of toluene an 8.96 ml (24.8 mmole) of 2.77N NaOH were mechanically stirred at -5° C., and 25.7 ml (49.6 mmole) of 1.93M phosgene in toluene was added dropwise over 30 minutes while maintaining -5°. After half the phosgene solution had been added, the rate of addition was increased easily. After stirring at -5° for an additional 30 minutes, the phases were separated and the toluene layer was dried over 10 g of solid sodium chloride. Concentration gave 5.5 g (98%) of dark yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05292726 |
| 出典データセット | uspto-grants-1994_03 |
| ORD ID | ord-9ca3b2c3f5464eb8817b2232083787af |
| 出典メモ | uspto-grants-1994_03 |