関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | Allyltrimethylsilane | HCID 69808 | — |
| 反応物 | 2-Fluoro-4-nitrobenzaldehyde | HCID 4562919 | — |
| 触媒 | Titanium Tetrachloride | HCID 24193 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-(2-Fluoro-4-nitro-phenyl)-3-buten-1-ol | HCID 23145779 | — |
反応手順
0.65 ml of titanium tetrachloride was added to a chloroform (12 ml) solution of 2.00 g of 4-nitro-2-fluoro-benzaldehyde produced according to the method described in U.S. Pat. No. 6,239,152, and the reaction liquid was stirred at room temperature for 10 minutes, and then 2.4 ml of allyl-trimethyl-silane was added to it, and the reaction liquid was stirred at room temperature for 20 minutes. The reaction liquid was diluted with ethyl acetate, washed with water and saturated saline, and dried with anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, and the residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=3/1) to obtain the entitled compound as an orange solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07728025B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-e409d2c505314342bc35b68cf061a516 |
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| 出典メモ | uspto-grants-2010_06 |
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