関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,6-Lutidine | HCID 7937 | — |
| 反応物 | 3,5-Dichlorobenzylic alcohol | HCID 43236 | — |
| 反応物 | Triisopropylsilyl trifluoromethanesulfonate | HCID 2724529 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | [(3,5-Dichlorobenzyl)oxy](triisopropyl)silane | HCID 11739096 | 79% |
反応手順
To a solution of (3,5-dichlorophenyl)methanol (10.0 g, 56.5 mmol) in methylene chloride (100 mL) at 0° C. was added 2,6-lutidine (16.4 mL, 141 mmol) followed by triisopropylsilyl triflate (19.7 mL, 73.4 mmol), and was stirred at 0° C. for 2 hours. The reaction was diluted with water and the organic layer was separated, washed with brine, dried over Na2SO4, filtered and concentrated. The residue was purified by chromatography on silica gel, eluting with hexane to provide the desired product (14.8 g, 79%). LC/MS: 333 (M+H)+, 1H NMR (CDCl3) δ 7.23 (s, 3H), 4.78 (s, 2H), 1.18 (m, 3H), 1.03 (s, 18H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08835423B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-f65339ddf077486e98d8dcd9eb97b4d8 |
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| 出典メモ | uspto-grants-2014_09 |
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