関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 4,7-dimethyl-1H-indene | HCID 81458 | — |
| 生成物 | Bis(4,7-dimethyl-2-indenyl)methane | HCID 11381059 | 44.1% |
反応手順
In a 500 mL flask equipped with magnetic stirring bar were introduced 10 g (0.069 moles) of 4,7-dimethyl-indene, 1.04 g (0.035 moles) of formalin and 2.64 g (0.014 moles) of para-toluenesulphonic acid in 100 ml of toluene; the mixture was heated to 80° C. and was maintained under stirring for 3 hours at 80° C. Then the reaction was quenched with water/NaHCO3; the conversion, measured by gas chromatographic analysis, was 82.4%. The organic layer was separated, washed with water and brought to dryness under reduced pressure. The crude product was crystallized upon standing at room temperature, and then was further purified by washing with pentane or MeOH, thus isolating 5.1 g of bis(4,7-dimethyl-2-indenyl)methane (purity of 90.2% by G.C.; yield=44.1%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06872863B2 |
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| 出典データセット | uspto-grants-2005_03 |
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| ORD ID | ord-b5374acbc004471ead25422deb1580ce |
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| 出典メモ | uspto-grants-2005_03 |
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