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Imidazole → tert-Butyl-dimethyl-(3-nitro-benzyloxy)-silane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| 反応物 | 3-Nitrobenzyl alcohol | HCID 69267 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | tert-Butyl-dimethyl-(3-nitro-benzyloxy)-silane | HCID 59428294 | 90% |
反応手順
A solution of compound 2 (4.7 g, 0.03 mol) and imidazole (2.71 g, 0.04 mol) in dry CH2Cl2 (30 mL) under N2 atmosphere at 0° C. was added a solution of TBDMS-Cl (5.08 g, 0.033 mol) in CH2Cl2 (15 mL) and allowed to stir at room temperature for 2 h. The precipitated solid was isolated by filtration and washed with CH2Cl2 (5×20 mL). The filtrate and combined CH2Cl2 fractions were dried over anhydrous Na2SO4 and concentrated under reduced pressure. The crude mass was purified by column chromatography (silica gel, eluant=3:7 mixture of ethyl acetate and hexane) to afford compound 3 (7.2 g, 90%) as a liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07939556B2 |
| 出典データセット | uspto-grants-2011_05 |
| ORD ID | ord-511748dbc83f4448af15c5ea3b65b0a4 |
| 出典メモ | uspto-grants-2011_05 |