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Dichloromethane → tert-Butyl 3-(((methylsulfonyl)oxy)methyl)pyrrolidine-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | tert-Butyl 3-(hydroxymethyl)pyrrolidine-1-carboxylate | HCID 5237175 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | tert-Butyl 3-(((methylsulfonyl)oxy)methyl)pyrrolidine-1-carboxylate | HCID 4183641 | 76.1% |
反応手順
Into the reaction flask was added tert-butyl 3-(hydroxymethyl)pyrrolidine-1-carboxylate (0.80 g, 4.0 mmol), methylene chloride (20 mL), and methanesulfonyl chloride (0.55 g, 4.8 mmol). The mixture was stirred at 0° C. when triethylamine (1.4 mL) was slowly added. The reaction mixture was stirred at rt for 2 h, followed by the addition of water (5 mL). The aqueous layer was extracted twice with methylene chloride. The combined organic layers were dried over Na2SO4, filtered and concentrated to give the desired product (0.85 g crude) which was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08871753B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-8389db3983d545ef8fc34a1650d12e97 |
| 出典メモ | uspto-grants-2014_10 |