참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 3-(Dimethylamino)pyrrolidine | HCID 2758519 | — |
| 반응물 | HCID 178489782 | HCID 178489782 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | HCID 178489786 | HCID 178489786 | 80% |
반응 단계
N,N-dimethylpyrrolidin-3-amine (114 mg, 1.00 mmol) was added to 5-chloro-N-[5-[2-(3,5-dimethoxyphenyl)ethyl]-2H-pyrazol-3-yl]pyrazine-2-carboxamide (136 mg, 0.35 mmol) in anhydrous dimethylsulfoxide (1.75 ml) at 25° C. The resulting solution was stirred at room temperature for 20 mins. The reaction mixture was diluted with methanol (5.00 ml) and the crude product was purified by ion exchange chromatography, using a SCX column. The desired product was eluted from the column using 7M NH3/MeOH and fractions were evaporated to dryness to afford impure product as a brown oil. The crude product 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 (130 mg, 80%) as a white 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-e73953707a8b4a1080dff2a6335102dd |
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| 출처 메모 | uspto-grants-2010_06 |
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