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Trifluoroacetic acid → hexahydro-2H-pyrazino[1,2-a]pyrazin-1(6H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | 1-(1,1-Dimethylethyl) 3-ethyl 4-[2-({[(1,1-dimethylethyl)oxy]carbonyl}amino)ethyl]-1,3-piperazinedicarboxylate | HCID 59215848 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | hexahydro-2H-pyrazino[1,2-a]pyrazin-1(6H)-one | HCID 45122044 | 38.6% |
反応手順
To a solution of 1-(1,1-dimethylethyl) 3-ethyl 4-[2-({[(1,1-dimethylethyl)oxy]carbonyl}amino)ethyl]-1,3-piperazinedicarboxylate (D77, 2.492 g, 6.21 mmol) in dichloromethane (30 mL) kept at 0° C. was added TFA (10 mL) dropwise. The solution was kept at 0° C. for 2 h, and then at room temperature for 6 h. The deprotected product was isolated by SCX and the resulting solution was evaporated at 50° C. to induce cyclization. The target product was purified by reverse phase chromatography (Oasis HLB 6 g×4 columns, eluted with water), obtaining 372 mg of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07683056B2 |
| 出典データセット | uspto-grants-2010_03 |
| ORD ID | ord-43ac294c0e8547e4b716fd4963c527a8 |
| 出典メモ | uspto-grants-2010_03 |