関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyldichlorosilane | HCID 6376 | — |
| 反応物 | Allyl acrylate | HCID 13835 | — |
| 触媒 | Phenothiazine | HCID 7108 | — |
| 触媒 | Triphenylphosphine | HCID 11776 | — |
| 生成物 | 3-(Dichloromethylsilyl)propyl 2-propenoate | HCID 9964588 | 68.3% |
反応手順
To a three-necked flask equipped as in Example 1 there was added 260 grams allylacrylate (2.32 moles), 0.5 grams catalyst prepared in accordance with U.S. Pat. No. 3,814,730 (2.6 weight percent Pt) and 1.04 grams phenothiazine. The mixture was heated with stirring to 65° C. and, using the vent of the condenser, purged with nitrogen. The heat source was then turned off and 237 grams (2.32 moles) CH3SiHCl2 was added dropwise, the temperature of the reaction mass being maintained at about 70° C. Upon completion of the addition of methyldichlorosilane the crude product was cooled to room temperature. One gram phenothiazine and 0.05 gram triphenyl phosphine were added to the product prior to distillation. Acryloxypropylmethyldichlorosilane (360 grams, 68% yield) was distilled at 109°-112° C./10 mm Hg.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04558111 |
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| 出典データセット | uspto-grants-1985_12 |
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| ORD ID | ord-cbb47104230840fbb54142cd61d56e4c |
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| 出典メモ | uspto-grants-1985_12 |
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