関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | N-(tert-Butoxycarbonyl)-D-prolinol | HCID 688279 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (R)-tert-Butyl 2-((tosyloxy)methyl)pyrrolidine-1-carboxylate | HCID 11760051 | 45% |
反応手順
A mixture of Boc-D-prolinol (201 mg, 1.0 mmol), p-toluenesulfonyl chloride (400 mg, 2.1 mmol), triethylamine (420 μL, 3.0 mmol), and 4-(dimethylamino)pyridine (12 mg, 0.1 mmol) in dichloromethane (10 mL) was heated at 40° C. for 48 hours, cooled to room temperature, concentrated under vacuum, diluted with ethyl acetate, washed with water and brine, dried (MgSO4), filtered, and concentrated. The residue was purified by column chromatography on silica gel to provide 160 mg (45%) of the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07456169B2 |
|---|
| 出典データセット | uspto-grants-2008_11 |
|---|
| ORD ID | ord-d63fff0499e247fd9dceeb7f7da20f56 |
|---|
| 出典メモ | uspto-grants-2008_11 |
|---|
