Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylformamide → 8-(6-amino-4-chloropyridin-2-ylamino)-6-chloro-N-(3-fluoropyridin-4-yl)imidazo[1,2-b]pyridazine-3-carboxamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 4-Chloropyridine-2,6-diamine | HCID 237847 | — |
| 반응물 | 8-Bromo-6-chloro-N-(3-fluoropyridin-4-yl)imidazo[1,2-b]pyridazine-3-carboxamide | HCID 59624495 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 8-(6-amino-4-chloropyridin-2-ylamino)-6-chloro-N-(3-fluoropyridin-4-yl)imidazo[1,2-b]pyridazine-3-carboxamide | HCID 59624351 | 78.8% |
반응 단계
To a solution of 4-chloropyridine-2,6-diamine (35.2 mg, 0.245 mmol) in THF (0.5 mL) was added 60% NaH (12.26 mg, 0.307 mmol). The mixture was stirred for 10 min. 5A (40 mg, 0.123 mmol) was added, followed by DMF (0.5 mL). The mixture was stirred at room temperature for 1 h. Water was added and the precipitated solid was collected by filtration, and dried to give crude 40A (42 mg, 59%). HPLC Rt=3.131 min (Chromolith SpeedROD 4.6×50 mm, 10-90% aqueous methanol containing 0.1% TFA, 4 min gradient, monitored at 220 nm), [M+H]=433.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08389527B2 |
| 출처 데이터셋 | uspto-grants-2013_03 |
| ORD ID | ord-f237d288611a4f8ca0d4b323f3981078 |
| 출처 메모 | uspto-grants-2013_03 |