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Sodium Chloride → Tert-butyl (3R)-3-(methanesulfonyloxy)pyrrolidine-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | tert-Butyl (3R)-3-hydroxypyrrolidine-1-carboxylate | HCID 6544479 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Tert-butyl (3R)-3-(methanesulfonyloxy)pyrrolidine-1-carboxylate | HCID 10934372 | — |
反応手順
16.91 ml of triethylamine and 9.36 ml of methanesulfonyl chloride were added, in that order, whilst ice-cooling, to a solution of 25 g of (3R)-1-t-butoxycarbonyl-3-hydroxypyrrolidine dissolved in 250 ml of dry tetrahydrofuran, and the mixture was stirred at 0° to 5° C. for 30 minutes and then at 15° C. for 30 minutes. At the end of this time, the mixture was poured into an aqueous solution of sodium chloride and extracted with ethyl acetate. The extract was washed with an aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate. The solvent was then removed by distillation under reduced pressure, to give 3.10 g of the title compound as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05242914 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-e65f24035a9c4030ba5dd6e5e6051a44 |
| 出典メモ | uspto-grants-1993_09 |