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Triethylamine → N,N'-di(tert-butyloxycarbonyl)-2-[3-(pyrid-2-yl)isoxazol-5-yl]pyrrolidine-1-carboximidamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1,3-Di-Boc-2-(trifluoromethylsulfonyl)guanidine | HCID 3694570 | — |
| 反応物 | 2-[3-(Pyrid-2-yl)isoxazol-5-yl]pyrrolidine | HCID 68813531 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N,N'-di(tert-butyloxycarbonyl)-2-[3-(pyrid-2-yl)isoxazol-5-yl]pyrrolidine-1-carboximidamide | HCID 68814905 | 76.2% |
反応手順
2-[3-(Pyrid-2-yl)isoxazol-5-yl]pyrrolidine (Method 12) (1.5 g, 7 mmol) was added to a solution of N,N′-di(tertbutyloxycarbonyl)-N″-(trifluoromethylsulphonyl)guanidine (2.59 g, 6.6 mmol) and triethylamine (0.975 ml) in DCM and the mixture stirred at ambient temperature for 8 hours. The mixture was then washed with water, dried (MgSO4) and the volatiles removed by evaporation. The residue was purified by chromatography on silica gel eluting with DCM/methanol (100:0 increasing in polarity to 98:2) to give the title compound (2.3 g, 70%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07579349B2 |
| 出典データセット | uspto-grants-2009_08 |
| ORD ID | ord-aac05e9011ea4aad9d3f54f9b185eb23 |
| 出典メモ | uspto-grants-2009_08 |