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Diethyl Ether → 4-(2',6'-Dimethoxyphenyl)-2-nitrobenzyl bromide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 4-(2',6'-Dimethoxyphenyl)-2-nitrobenzyl alcohol | HCID 70056006 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(2',6'-Dimethoxyphenyl)-2-nitrobenzyl bromide | HCID 22452118 | — |
反応手順
To a solution of 1.8 g (6.23 mmol) of 4-(2′,6′-dimethoxyphenyl)-2-nitrobenzyl alcohol and 2.3 g (8.72 mmol) of Ph3P in CH2Cl2 (20 mL) at 0° C. was added 1.32 g (7.5 mmol) of NBS. The reaction mixture was stirred at 0° C. for 30 min at which time TLC analysis (eluted with 25% Et2O in hexanes) indicated that the starting material had been consumed. The reaction mixture was concentrated and the crude residue was purified by flash column chromatography on silica gel eluted with 50% Et2O in hexanes to give 4-(2′,6′-dimethoxyphenyl)-2-nitrobenzyl bromide as a pale yellow solid. Trituration with hexanes gave the product as a white 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-ce7d3c1d5e7e469d8f1217d26e5b77e2 |
| 出典メモ | uspto-grants-2002_06 |