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Sodium hydride → 3-(3-amino4-chloro-6-fluoro-2-methoxyphenyl)-6-trifluoromethyl-2,4-(1H,3H)-pyrimidinedione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 反応物 | Ethyl 3-amino-4,4,4-trifluorocrotonate | HCID 5702529 | — |
| 反応物 | ethyl N-(3-amino4-chloro-6-fluoro-2-methoxyphenyl)carbamate | HCID 18315064 | — |
| 反応物 | Sodium trimethylsilanolate | HCID 23672319 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-(3-amino4-chloro-6-fluoro-2-methoxyphenyl)-6-trifluoromethyl-2,4-(1H,3H)-pyrimidinedione | HCID 18315080 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06352958B1 |
| 出典データセット | uspto-grants-2002_03 |
| ORD ID | ord-b0d1e0b5359340c1aa863386b79bc1a2 |
| 出典メモ | uspto-grants-2002_03 |