関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Iodoform | HCID 6374 | — |
| 反応物 | Difluoro-4-chlorophenylacetaldehyde | HCID 23237846 | — |
| 触媒 | chromium(II) dichloride | HCID 10197677 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1,1-Difluoro-1-(4-chlorophenyl)-3-iodo-2-propene | HCID 54422725 | — |
反応手順
Under a nitrogen atmosphere, a stirred suspension of 29.5 grams (0.24 mole) of anhydrous chromium(II) dichloride in 400 mL of tetrahydrofuran is cooled to 0° C., and a solution of 7.6 grams (0.04 mole) of difluoro-4-chlorophenylacetaldehyde and 31.5 grams (0.08 mole) of iodoform in 200 mL of tetrahydrofuran is added dropwise. Upon completion of addition, the reaction mixture is stirred at 0° C. for three hours. After this time the reaction mixture is poured into about 1200 mL of water, and the mixture is extracted with three 150 mL portions of diethyl ether. The combined extracts are dried with sodium sulfate and filtered. The filtrate is concentrated under reduced pressure, yielding 1,1-difluoro-1-(4-chlorophenyl)-3-iodo-2-propene.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05622954 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-f7b1f32886c146759c5c2f973d915276 |
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| 出典メモ | uspto-grants-1997_04 |
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