참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | rel-(2R,6S)-2,6-dimethylpiperazine | HCID 6950261 | — |
| 반응물 | HCID 178489782 | HCID 178489782 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | HCID 178489798 | HCID 178489798 | 35.2% |
반응 단계
(2S,6R)-2,6-Dimethylpiperazine (228 mg, 2.00 mmol) was added in one portion to 5-chloro-N-[5-[2-(3,5-dimethoxyphenyl)ethyl]-2H-pyrazol-3-yl]pyrazine-2-carboxamide (388 mg, 1.00 mmol) in anhydrous dimethylsulfoxide (1.00 ml) at 25° C. The resulting solution was stirred at 100° C. for 18 h. The crude product was purified by ion exchange chromatography, using an SCX column. The desired product was eluted from the column using 7M NH3/MeOH to afford impure material. The concentrated eluent was purified by preparative HPLC, using decreasingly polar mixtures of water (containing 1% NH3) and MeCN as eluents. Fractions containing the desired compound were evaporated to dryness to afford the title compound (164 mg, 35%) as a cream solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07737149B2 |
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| 출처 데이터셋 | uspto-grants-2010_06 |
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| ORD ID | ord-f3403cefc69c4b158649f4ab3d6f009a |
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| 출처 메모 | uspto-grants-2010_06 |
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