関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 2-Bromopropan-1-ol | HCID 11713 | — |
| 反応物 | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| 生成物 | (3-Bromopropoxy)(tert-butyl)dimethylsilane | HCID 607486 | — |
反応手順
Separately, 7.0 g (corresponding to 50.4 mmol) of 2-bromopropanol and 6.86 g (corresponding to 101 mmol) of imidazole were dissolved in 50 mL of dimethylformamide, and cooled to 0° C. Then, 7.59 g (corresponding to 50.4 mmol) of t-butyldimethylchlorosilane was added thereto. After the reaction mixture was stirred at room temperature for 24 hours, it was supplemented with a saturated sodium chloride aqueous solution, and extracted three times with diethyl ether. The combined diethyl ether layers were dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The resulting crude product was purified by vacuum distillation (100° C., 70 mmHg), to obtain 7.23 g (corresponding to 30.2 mmol) of 1-bromo-3-(t-butyldimethylsiloxy)propane (FIG. 10, Step 3).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08207189B2 |
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| 出典データセット | uspto-grants-2012_06 |
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| ORD ID | ord-ad77c0c3e941425d86af4d13ba573f7f |
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| 出典メモ | uspto-grants-2012_06 |
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