참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 1-Bromohexane | HCID 8101 | — |
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | 2,3-Dicyanohydroquinone | HCID 78467 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 3-(Hexyloxy)-6-hydroxybenzene-1,2-dicarbonitrile | HCID 15006689 | 31.8% |
반응 단계
27 g (168.8 mM) of 2,3-dicyanohydroquinone and 22.2 g (337 mM) of 85%-potassium hydroxide were dissolved in a mixture solvent of 65 ml of methanol and 302 ml of dimethylformamide, followed by heating to 50° C. To the solution, 33.4 g (202.4 mM) of hexyl bromide were added dropwise in 25 minutes, followed by heating to 100° C. and stirring for 3 hours. The reaction mixture was poured into cold water and washed with ether. The water layer was acidified with 6N-hydrochloric acid to provide a pH value of 1, followed by precipitation of a crystal. The crystal was extracted with ether, and the ether layer was washed with 5%-sodium hydrogen-carbonate aqueous solution and further washed with water, followed by distilling-off of the solvent to obtain a crude product. The crude product was treated with activated carbon and recrystallized from methanol to obtain 13.1 g of 2,3-dicyano-4-hexyloxyphenol.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05858269 |
|---|
| 출처 데이터셋 | uspto-grants-1999_01 |
|---|
| ORD ID | ord-756d7f0ce9f147b88b64f84023cc62fd |
|---|
| 출처 메모 | uspto-grants-1999_01 |
|---|