関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Oxygen | HCID 977 | — |
| 反応物 | Acetylacetone | HCID 31261 | — |
| 反応物 | Benzene, 1,1'-oxybis[4-methyl- | HCID 74098 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 生成物 | 2,8-Dimethyldibenzofuran | HCID 639319 | 17.5% |
反応手順
15 g of 4,4'-dimethyldiphenyl ether, 0.034 g (0.15 m. mole) of palladium acetate and 0.015 g (0.15 m. mole) of acetylacetone were placed in a glass vessel and this is placed in a 100 ml-autoclave. Then a mixture gas of nitrogen and oxygen of molar ratio 1:1 was filled in it to 50 kg/cm2 of inner pressure. The autoclave was shaken at 150° C. for 5 hours. After completion of the reaction, the reaction mixture was subjected to fractional distillation. After distilling out the unreacted 4,4'-dimethyldiphenyl ether, a distillate having b.p. 130°-135° C./12 mmHg was recrystallized from ethanol to give 2.6 g (13 m. moles) of 2,8-dimethyldibenzofuran. The obtained 2,8-dimethylbenzofuran showed m.p. 62°-64° C. (reference value, 64° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04042603 |
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| 出典データセット | uspto-grants-1977_08 |
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| ORD ID | ord-97e93d0900fa4ab98641e73a54e603f6 |
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| 出典メモ | uspto-grants-1977_08 |
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