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Triphenylphosphine → 1-(1-Trifluoromethylprop-1-en-3-yloxy)-2-bromo-4-fluorobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| 反応物 | 2-Bromo-4-fluorophenol | HCID 605472 | — |
| 反応物 | 4,4,4-Trifluoro-2-buten-1-ol | HCID 2777076 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(1-Trifluoromethylprop-1-en-3-yloxy)-2-bromo-4-fluorobenzene | HCID 53921978 | 120.1% |
反応手順
A solution of 2.10 gm (16.7 mMol) 1-trifluoromethylprop-1-en-3-ol, 3.19 gm (16.7 mMol) 2-bromo-4-fluorophenol, and 4.81 gm (18.4 mMol) triphenylphosphine in 25 mL dichloromethane was cooled to 0° C. and then 2.9 mL (18.4 mMol) diethyl azodicarboxylate were added. The reaction mixture was stirred for 1 hour at room temperature and then the reaction mixture was directly subjected to flash silica gel chromatography, eluting with 20:1 hexane:ethyl acetate. Fractions containing product were combined and concentrated under reduced pressure to provide 6 gm of crude 1-(1-trifluoromethylprop-1-en-3-yloxy)-2-bromo-4-fluorobenzene.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06881733B1 |
| 出典データセット | uspto-grants-2005_04 |
| ORD ID | ord-abfd6120e19141a8b130608e42b5b89d |
| 出典メモ | uspto-grants-2005_04 |