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Imidazole → (R)-5-(((tert-Butyldimethylsilyl)oxy)methyl)pyrrolidin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| 反応物 | (R)-(-)-5-(Hydroxymethyl)-2-pyrrolidinone | HCID 7128291 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | (R)-5-(((tert-Butyldimethylsilyl)oxy)methyl)pyrrolidin-2-one | HCID 13771167 | 107.5% |
反応手順
Under atmosphere of argon, a solution of (5R)-5-hydroxymethylpyrollidin-2-one (10 g) and imidazole (8.8 g) in dry dimethylformamide (50 mL) was added by a solution of t-butyldimethylsilyl chloride (15.6 g) in dry dimethylformamide (50 mL) at room temperature, and the mixture was stirred for 5 hours. To the mixture, a mixed solvent of ethyl acetate and hexane was added. The diluted solution was washed with water and brine successively, dried over an anhydrous sodium sulfate, concentrated under reduced pressure to give the title compound (21.41 g) having the following physical data.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08207223B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-a03349e921f9436080d515cb9d94a4c2 |
| 出典メモ | uspto-grants-2012_06 |