참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Cyanide | HCID 9032 | — |
| 반응물 | 1-(3-Amino-4,5-dimethoxyphenyl)ethanone | HCID 21459185 | — |
| 반응물 | Sodium Nitrite | HCID 23668193 | — |
| 반응물 | HCID 178418546 | HCID 178418546 | — |
| 용매 | Hydrochloric Acid | HCID 313 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 5-Acetyl-2,3-dimethoxybenzonitrile | HCID 21458980 | — |
반응 단계
A solution of 5.2 g of sodium nitrite in 20 ml of water is added dropwise at 0° within 20 minutes to 14.0 g of 5'-amino-3',4'-dimethoxyacetophenone dissolved in 155 ml of 1N hydrochloric acid. After stirring at -2° for 30 minutes the cold diazonium salt solution is added dropwise within 30 minutes at 5°-10° to a solution of 8.7 g of copper(I) cyanide and 5.45 g of potassium cyanide in 60 ml of water. After completion of the addition 200 ml of methylene chloride are added, and the reaction mixture is stirred at 23° for 3 hours and then filtered. The organic phase is separated, washed with water, dried over sodium sulfate and evaporated. The residue is recrystallized from methylene chloride/petroleum ether. There is obtained 5'-cyano-3',4'-dimethoxyacetophenone of m.p. 125°-126°.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05633371 |
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| 출처 데이터셋 | uspto-grants-1997_05 |
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| ORD ID | ord-1d614496fe8746eaa68466ab7c4f69d3 |
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| 출처 메모 | uspto-grants-1997_05 |
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