反应详情

温度

0 °C

The product from Step 1 (2.5 g) was dissolved in dry THF (50 ml) and the flask purged with nitrogen. Sodium bis-trimethylsilylamide (22.1 ml of a 1M solution in THF) was added dropwise with stirring at 0° C. A yellow precipitate appeared, and the reaction was stirred for 3 hours at 0° C. The reaction was quenched with concentrated hydrochloric acid (5 ml) at 0° C. and then poured onto ice water, extracted with DCM and dried over magnesium sulphate. The solvent was evaporated to give 3-(2,4,6-trifluorophenyl)-1H-pyrido[2,3-d]pyridazine-2,4-dione as a yellow solid. Further product crystallised out of the aqueous solution overnight, to give a total yield of 1.29 g, m.p. >300° C.

1. customthe flask purged with nitrogen
2. additionSodium bis-trimethylsilylamide (22.1 ml of a 1M solution in THF) was added dropwise
3. stirringthe reaction was stirred for 3 hours at 0° C
4. customThe reaction was quenched with concentrated hydrochloric acid (5 ml) at 0° C.
5. additionpoured onto ice water
6. extractionextracted with DCM
7. dry with materialdried over magnesium sulphate
8. customThe solvent was evaporated