Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Urea → 6-(2,4-Difluoro-phenoxy)-1H-pyrido[3,4-d]pyrimidine-2,4-dione
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Urea | HCID 1176 | — |
| 반응물 | 5-Amino-2-(2,4-difluoro-phenoxy)-isonicotinic acid methyl ester | HCID 58820193 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 6-(2,4-Difluoro-phenoxy)-1H-pyrido[3,4-d]pyrimidine-2,4-dione | HCID 18440625 | 98.6% |
반응 단계
Compound (1C) (4.2 g, 15.0 mmol) and urea (9.0 g, 10 eq) were heated to a melt at 160° C. with stirring. After 2 hours, the melt solidified and by TLC the reaction was complete. The reaction mixture was cooled to room temperature, water (250 mL) was added, and the resulting mixture was left to stand for 1 hour. Then the solids were broken up with a spatula and the mixture was stirred vigorously for 1 hour. After suction filtration, a tan powder was collected which was air-dried in the frit for two days. Drying under high vacuum at 56° C. gave the title compound (1D) as a tan powder (4.307 g, (M−H)−=290, M.P.>300° C.).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07189731B2 |
| 출처 데이터셋 | uspto-grants-2007_03 |
| ORD ID | ord-b22efac00e8b497f82147eca830e8a3b |
| 출처 메모 | uspto-grants-2007_03 |