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Methyl 4-(bromomethyl)benzoate → HCID 18510220、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl 4-(bromomethyl)benzoate | HCID 256687 | — |
| 反応物 | Tetrabutylammonium Fluoride | HCID 2724141 | — |
| 反応物 | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| 反応物 | 2-(4-Fluorophenyl)-2-[(trimethylsilyl)oxy]acetonitrile | HCID 11715552 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 18510220 | HCID 18510220 | 65.6% |
反応手順
To 2-(4-fluorophenyl)-2-[(trimethylsilyl)oxy]acetonitrile (0.500 g, 2.24 mmol) in degassed THF (11 ml) at −78° C. was added LHMDS 1M in THF (2.4 ml). To the previous reaction mixture a solution of methyl 4-(bromomethyl)benzoate (0.513 g, 2.25 mmol) in THF (2 ml) was then added. After a period of 1 h at r.t., tetrabutylammonium fluoride solution 1 M in THF (2.23 ml) was added to the reaction mixture and stirred for 10 minutes. Water was added and the mixture was extracted with ethyl acetate. The organic phase was dried over sodium sulfate and evaporated to dryness. The residue was purified by flash chromatography using hexane/ethyl acetate 30% giving 0.4 g of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06583126B2 |
| 出典データセット | uspto-grants-2003_06 |
| ORD ID | ord-8d0496ff676b429dbd0e273701dac41f |
| 出典メモ | uspto-grants-2003_06 |