関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Tert-butyl-(3-iodopropoxy)-dimethylsilane | HCID 11022956 | — |
| 反応物 | 1-(3,4,5-Trimethoxybenzyl)-2-oxopyrrolidine | HCID 18464662 | — |
| 反応物 | CID 53628100 | HCID 178418400 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 1-(3,4,5-Trimethoxybenzyl)-3-(3-(t-butyldimethylsilyloxy)propyl)-2-oxopyrrolidine | HCID 22009451 | — |
反応手順
Combine 1-(3,4,5-trimethoxybenzyl)-2-oxopyrrolidine (0.84 g, 3.16 mmol) and tetrahydrofuran (10 mL). Cool to −78° C. using a dry-ice/acetone bath. Add a solution of sec-butyl lithium (2.56 mL, 1.3 M in hexane, 3.33 mmol). After 30 minutes, add 3-(t-butyldimethylsilyloxy)propyl iodide (1.0 g, 3.33 mmol). After the addition is complete, warm to ambient temperature. After 2 hours, add water and extract three times with ethyl acetate. Dry the combined organic layers over Na2SO4, filter, and concentrate in vacuo to obtain a residue. Chromatograph the residue on silica gel eluting with ethyl acetate to give the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06211199B1 |
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| 出典データセット | uspto-grants-2001_04 |
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| ORD ID | ord-cc292f7d6f9a45dc8e9ce1f2816341bd |
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| 出典メモ | uspto-grants-2001_04 |
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