Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Pyridine → 3,5-Dimethyl-isoxazole-4-carboxylic acid [2-methyl-6-((2S,3'R)-2-methyl-[1,3']bipyrrolidinyl-1'-yl)-pyridin-3-yl]-amide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | Tris(hydroxymethyl)aminomethane | HCID 6503 | — |
| 반응물 | 3,5-Dimethylisoxazole-4-carbonyl Chloride | HCID 2736265 | — |
| 반응물 | 2-methyl-6-[(3R)-3-[(2S)-2-methylpyrrolidin-1-yl]pyrrolidin-1-yl]pyridin-3-amine | HCID 67480461 | — |
| 용매 | 1,2-Dichloroethane | HCID 11 | — |
| 생성물 | 3,5-Dimethyl-isoxazole-4-carboxylic acid [2-methyl-6-((2S,3'R)-2-methyl-[1,3']bipyrrolidinyl-1'-yl)-pyridin-3-yl]-amide | HCID 54597156 | 35.9% |
반응 단계
To a solution of 2-methyl-6-[(3R)-3-[(2S)-2-methylpyrrolidin-1-yl]pyrrolidin-1-yl]pyridin-3-amine (22.7 mg, 0.09 mmol) in DCE (1 mL) was added pyridine (0.22 mL, 2.7 mmol) followed by a solution of 3,5-dimethyl-isoxazole-4-carbonyl chloride (43 mg, 0.27 mmol) in DCE (1 mL) and stirred at ambient temperature for 5 hours. To this mixture was then added trisamine resin (200 mg, 0.8 mmol, 4 mmol/g loading), stirred for 30 min, filtered and concentrated to afford a crude solid which was purified by flash column chromatography (5% 7N NH3 in MeOH/CH2Cl2) to obtain 12.4 mg of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08859588B2 |
| 출처 데이터셋 | uspto-grants-2014_10 |
| ORD ID | ord-df017cd31ca74dc7a4ea446d02557373 |
| 출처 메모 | uspto-grants-2014_10 |