関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trimethoxysilane | HCID 17215 | — |
| 反応物 | Allyl 3,4-methylenedioxy-6-nitrobenzyl ether | HCID 21941062 | — |
| 触媒 | Platinic chloride hexahydrate | HCID 134756 | — |
| 生成物 | 4,5-Methylenedioxy-2-nitrobenzyl 3-(trimethoxysilyl)propyl ether | HCID 21941039 | 52.4% |
反応手順
A 10-ml eggplant type flask was purged with nitrogen, and charged with 1.0 g (4.2 mmol) of allyl 3,4-methylenedioxy-6-nitrobenzyl ether, 0.616 g (5 mmol) of trimethoxysilane, and an infinitesimal amount of hydrogen hexachloroplatinate(IV) hexahydrate (H2PtCl6·6H2O), followed by stirring at 37° C. for 30 minutes. Thereafter, the bath temperature was raised to 100° C., and the reaction was completed in 2 hours. The reaction mixture was purified by silica gel column chromatography using a medium-pressure column. Using a mixture of hexane, ethyl acetate and tetramethoxysilane (in a volume ratio of 100:20: 1) as the eluent, 0.80 g (2.2 mmol) of the desired product was obtained in a 52% yield. Its Rf value (for the aforesaid eluent) was 0.1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07112397B2 |
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| 出典データセット | uspto-grants-2006_09 |
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| ORD ID | ord-8b6f05fc079d4e6cba0e3779d2c364df |
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| 出典メモ | uspto-grants-2006_09 |
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