Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium hydride → 3-(3-amino4-chloro-6-fluoro-2-methoxyphenyl)-6-trifluoromethyl-2,4-(1H,3H)-pyrimidinedione
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 반응물 | Ethyl 3-amino-4,4,4-trifluorocrotonate | HCID 5702529 | — |
| 반응물 | ethyl N-(3-amino4-chloro-6-fluoro-2-methoxyphenyl)carbamate | HCID 18315064 | — |
| 반응물 | Sodium trimethylsilanolate | HCID 23672319 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 3-(3-amino4-chloro-6-fluoro-2-methoxyphenyl)-6-trifluoromethyl-2,4-(1H,3H)-pyrimidinedione | HCID 18315080 | — |
반응 단계
This compound was prepared using 4.0 grams (0.036 mole) of sodium trimethylsilanolate, 6.6 grams (0.036 mole) of ethyl 3-amino4,4,4-trifluorocrotonate, 8.5 grams (0.032 mole) of ethyl N-(3-amino4-chloro-6-fluoro-2-methoxyphenyl)carbamate, and 2.2 grams (0.014 mole) of DBU in 75 mL of DMF. This preparation differs from well-known literature preparations for pyrimidinedione rings in that sodium trimethylsilanolate and DBU were used rather than sodium hydride. The yield of title compound was 1.7 grams. The NMR spectrum was consistent with the proposed structure.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06352958B1 |
| 출처 데이터셋 | uspto-grants-2002_03 |
| ORD ID | ord-b0d1e0b5359340c1aa863386b79bc1a2 |
| 출처 메모 | uspto-grants-2002_03 |