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Carbon Tetrachloride → 1-(Chloromethyl)-3,5-bis(trifluoromethyl)benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Carbon Tetrachloride | HCID 5943 | — |
| 反応物 | Pentane | HCID 8003 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 3,5-Bis(trifluoromethyl)benzyl alcohol | HCID 122933 | — |
| 生成物 | 1-(Chloromethyl)-3,5-bis(trifluoromethyl)benzene | HCID 123576 | 59% |
反応手順
Triphenylphosphine (371 mg, 1.41 mmol) was added to a solution of 3,5-bistrifluoromethylbenzyl alcohol (257 mg, 1.05 mmol) in dry CCl4 (2 ml). The mixture was refluxed for 1 h, then cooled to room temp. Pentane (2 ml) was added, and the mixture stirred for a further 5 min., then filtered. The solid was washed with pentane (2 ml), and the filtrate concentrated in vacuo. The crude product was purified by column chromatography [SiO2: hexane-ethyl acetate 4:1] to give 3,5-bistrifluoromethylbenzyl chloride (162 mg, 59%); TLC (hexane-ethyl acetate 1:1) rf=0.73.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05760248 |
| 出典データセット | uspto-grants-1998_06 |
| ORD ID | ord-91e2fcaf04b64c868c7f232e5e96d6f5 |
| 出典メモ | uspto-grants-1998_06 |