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Nitrogen → 2-Chloro-4-methoxy-1-nitrobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitrogen | HCID 947 | — |
| 反応物 | Dimethyl Sulfate | HCID 6497 | — |
| 反応物 | 3-Chloro-4-nitrophenol | HCID 10283 | — |
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 生成物 | 2-Chloro-4-methoxy-1-nitrobenzene | HCID 593789 | 72.4% |
反応手順
In an atomosphere of N2 were added to a stirred suspension of 31 g NaH in 2.2 l anhydrous THF 199.5 g (1.15 mole) 3-chloro-4-nitrophenol (3). This was followed by the addition of dimethylsulfate (575 ml). The whole mixture was heated under reflux during 1.5 h. After cooling, it was poured into a cold (0° C.) diluted NH4OH solution, to destroy the excess of dimethylsulfate, and stirred for two hours. The product was isolated by extraction with diethylether. The ethereal extracts were dried with MgSO4 and evaporated at reduced pressure affording 156 g (72.4%) of 3-chloro-4-nitroanisole.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05079257 |
| 出典データセット | uspto-grants-1992_01 |
| ORD ID | ord-9c079650b12644a199ff07f60105eabf |
| 出典メモ | uspto-grants-1992_01 |