Sodium bis(trimethylsilyl)amide → 6-(2,4,6-Trifluorophenyl)pyrido[2,3-c]pyridazine-5,7(6H,8H)-dione
反応式
C(O[C:4]([C:6]1[CH:11]=[CH:10][N:9]=[N:8][C:7]=1[NH:12][C:13](=[O:24])[CH2:14][C:15]1[C:20]([F:21])=[CH:19][C:18]([F:22])=[CH:17][C:16]=1[F:23])=[O:5])C.C[Si]([N-][Si](C)(C)C)(C)C.[Na+]>C1COCC1>[F:21][C:20]1[CH:19]=[C:18]([F:22])[CH:17]=[C:16]([F:23])[C:15]=1[CH:14]1[C:13](=[O:24])[NH:12][C:7]2[N:8]=[N:9][CH:10]=[CH:11][C:6]=2[C:4]1=[O:5]参加物
4
反応条件
- 温度
- 0 °C
実験手順
The product from Step 2 (2.0 g) was dissolved in dry THF (50 ml), and sodium bis-trimethylsilylamide (17.7 ml of a 11.0M solution in THF) was added dropwise with stirring under nitrogen at 0° C. The reaction was stirred for 3 hours at 0° C. and a yellow precipitate was formed. The reaction was quenched with concentrated hydrochloric acid and then poured into ice water. The solid was filtered, washed with water and air dried to give 6-(2,4,6-trifluorophenyl)-8H-pyrido[2,3-c]pyridazine-5,7-dione as a yellow solid (1.9 2 g), m.p. >330° C., still containing some THF, which was used without further purification.