関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfate | HCID 6497 | — |
| 反応物 | 4,4'-Dihydroxybiphenyl | HCID 7112 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-Hydroxy-4'-methoxybiphenyl | HCID 11030839 | 48% |
反応手順
120 ml of water and sodium hydroxide (14.00 g, 0.35 mol) were placed in a conical flask and dissolved. 4,4'-Dihydroxybiphenyl (28.00 g, 0.15 mol) was then added and heated to reflux for 2 hours with stirring using a condenser. Dimethyl sulfate (14.5 ml, 0.15 mol) was added dropwise over about 40 minutes. After addition, the mixture was heated while stirring for 2 hours, and then allowed to cool and filtrated. The filter cake was transferred into 700 ml of water, which was then heated to boiling temperature, and filtrated while still keeping warm. The filtrate was kept at 70° C., and 20% hydrochloric acid was added. White precipitation: formed was washed extensively. Recrystallization from ethanol yielded 4'-methoxy-4-hydroxybiphenyl (13.17 g, Yield: 48.0%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05412079 |
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| 出典データセット | uspto-grants-1995_05 |
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| ORD ID | ord-22bc116db45d424b96b7e0d2b5e88843 |
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| 出典メモ | uspto-grants-1995_05 |
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