Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 63758생성일: 2026년 10월 24일
Cyclooctylamine → n-Cyclooctyl-5-phenyl-7-(trifluoromethyl)-4,5,6,7-tetrahydropyrazolo[1,5-a]pyrimidine-3-carboxamide
https://huagongshe.com/ko/reaction/63758
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Cyclooctylamine | HCID 2903 | — |
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 반응물 | 4,4,4-Trifluoro-1-phenyl-1,3-butanedione | HCID 67589 | — |
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 촉매 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Sodium Bicarbonate | HCID 516892 | — |
| 생성물 | n-Cyclooctyl-5-phenyl-7-(trifluoromethyl)-4,5,6,7-tetrahydropyrazolo[1,5-a]pyrimidine-3-carboxamide | HCID 136071210 | 96% |
반응 단계
Cyclooctylamine (24 mg, 0.19 mmol) was added to a suspension of compound 1 (0.05 g, 0.16 mmol), WSC (37 mg, 0.19 mmol), HOBt (29 mg, 0.19 mmol) and DMAP (23 mg, 0.19 mmol) in DMF (1.5 mL). The reaction mixture was stirred at room temperature for 14 h, diluted with DCM (0.5 mL) and saturated NaHCO3 solution (0.5 mL), and then separated using PHASE-SEP filtration syringe. The organic layer was concentrated and loaded onto preparative HPLC (Gilson 215 system). The purest fractions were combined to give 64.6 mg (96% yield) of the title compound as a white solid. Reverse Phase LC/MS: CAPCELLPAKCC18UG120, S-3 μm, 2.0×50 mm, UV detection at 220, 8 min. gradient 10-100% Solvent B/A (Solvent A: CH3CN with 0.1% TFA, Solvent B: H2O with 0.1% TFA), 0.5 mL/min. Rt=1.90 min, (96% pure). MS (M+H: 421).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09447100B2 |
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| 출처 데이터셋 | uspto-grants-2016_09 |
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| ORD ID | ord-53bd5970fa194c108b523c674152c0cb |
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| 출처 메모 | uspto-grants-2016_09 |
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