関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 3,5-Dimethylphenol | HCID 7948 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3,5-Dimethyl-4-nitrophenol | HCID 138466 | — |
| 生成物 | 3,5-Dimethyl-4-nitrosophenol | HCID 236019 | 143.3% |
反応手順
[3,5-Dimethyl-4-nitrophenol was synthesized by the reference procedures (U.S. Pat. No. 4,564,640)] 750 ml of Concentrated hydrochloric acid was added to a solution of 3,5-dimethylphenol (80.6 g) in 750 ml of 95% ethanol. The mixture was cooled to 0° C. in an ice/methanol bath. While maintaining the temperature of the reaction mixture below 5° C., a solution of NaNO2 (69.0 g) in 150 ml of water was added dropwise to the reaction mixture. The mixture was stirred at 0° C. for more than an hour and then poured into 9 liters of water. The aqueous mixture was filtered to give a yellow solid which was recrystallized from hot methanol and filtered to give 71.45 g of 3,5-dimethyl-4-nitrosophenol as a yellow solid. Mp. 180-181° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08188314B2 |
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| 出典データセット | uspto-grants-2012_05 |
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| ORD ID | ord-351be53f9c6f4d8d841ff848abc0b407 |
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| 出典メモ | uspto-grants-2012_05 |
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