반응 #68609

반응 방정식

hydrazine hydrate

(6-phenylimidazo[1,2-b]pyridazin-3-yl)(quinolin-6-yl)methanone

KOH

diethylene glycol

→

6-((6-Phenylimidazo[1,2-b]pyridazin-3-yl)methyl)quinoline

용매

water

반응 조건

후처리

1. 1
   기타sealed
2. 2
   추출extracted with DCM (2×75 mL)
3. 3
   세척The combined organics were washed with brine (75 mL)
4. 4
   건조dried with MgSO4
5. 5
   여과filtered
6. 6
   농축concentrated
7. 7
   기타to give a brown solid
8. 8
   기타purified by prep HPLC
9. 9
   기타to give the product as the formic acid salt

실험 절차

A 10-20 mL microwave vial was charged with hydrazine hydrate (0.0312 ml, 0.642 mmol), (6-phenylimidazo[1,2-b]pyridazin-3-yl)(quinolin-6-yl)methanone (0.150 g, 0.428 mmol), KOH (0.0961 g, 1.71 mmol), and diethylene glycol (4.09 ml, 42.8 mmol), sealed, then placed in a Personal Chemistry microwave at 130° C. for 20 minutes after a 5 minute pre-stir. The mixture was diluted with water (75 mL), then extracted with DCM (2×75 mL). The combined organics were washed with brine (75 mL), then dried with MgSO4, filtered, and concentrated to give a brown solid, then purified by prep HPLC to give the product as the formic acid salt. MS (ESI pos. ion) m/z: 337 (MH+). Calc'd exact mass for C22H16N4: 336.

출처