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Cesium carbonate → 4-(2',6'-Dimethoxyphenyl)-2-nitrobenzyl alcohol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Tricyclohexylphosphine | HCID 75806 | — |
| 反応物 | 4-Chloro-2-nitrobenzyl alcohol | HCID 89956 | — |
| 反応物 | (2,6-Dimethoxyphenyl)boronic acid | HCID 2734343 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 4-(2',6'-Dimethoxyphenyl)-2-nitrobenzyl alcohol | HCID 70056006 | — |
反応手順
A mixture of 5.0 g (26.7 mmol) of 2-nitro-4-chlorobenzyl alcohol, 6.33 g (34.8 mmol) of 2,6-dimethoxybenzene boronic acid, 0.73 g (0.80 mmol) of Pd2dba3, 11.3 g (34.8 mmol) of Cs2CO3, and 0.45 g (1.60 mmol) of Cy3P was dissolved in 100 mL of dioxane and warmed to reflux for 18 h. The reaction mixture was cooled, filtered through a pad of silica gel which was washed with Et2O and concentrated. The residue was purified by flash column chromatography on silica gel eluted with a gradient of 25-50% Et2O in hexanes and gave 4-(2′,6′-dimethoxyphenyl)-2-nitrobenzyl alcohol as a pale yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06403584B1 |
| 出典データセット | uspto-grants-2002_06 |
| ORD ID | ord-8bf5fae181a84a2da0e6ddfa8142ed82 |
| 出典メモ | uspto-grants-2002_06 |