Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → (2S)-2-methyl-1-[(2-methyl-4-pyridinyl)carbonyl]-4-{[4-(trifluoromethyl)phenyl]sulfonyl}piperazine formic acid salt
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1) | HCID 2733084 | — |
| 반응물 | 2-Methylpyridine-4-carboxylic acid | HCID 2762821 | — |
| 반응물 | (S)-3-Methyl-1-((4-(trifluoromethyl)phenyl)sulfonyl)piperazine | HCID 59152086 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | (2S)-2-methyl-1-[(2-methyl-4-pyridinyl)carbonyl]-4-{[4-(trifluoromethyl)phenyl]sulfonyl}piperazine formic acid salt | HCID 44612081 | 120.7% |
반응 단계
To a solution of (3S)-3-methyl-1-{[4-(trifluoromethyl)phenyl]sulfonyl}piperazine (Description 2) (80 mg, 0.259 mmol) in DMF (5 ml) was added 2-methyl-4-pyridinecarboxylic acid (35.6 mg, 0.259 mmol), HOBT.H2O (39.7 mg, 0.259 mmol), HBTU (98 mg, 0.259 mmol) and DIPEA (0.136 ml, 0.778 mmol) and the reaction mixture was stirred at room temperature overnight. DMF was evaporated in vacuo then DCM (5 ml) was added and washed with saturated aq. NaHCO3 solution (5 ml), dried on a phase separation cartridge and evaporated in vacuo. The crude material was dissolved in MeCN/DMSO 1:1 and purified by MDAP. The desired fractions were collected and concentrated in vacuo giving the title compound (74 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08530478B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-43d2502aae1d4b49bf668f12fc6946c8 |
| 출처 메모 | uspto-grants-2013_09 |