반응 #684968
ord-d558389e953e49db9fe05adf4d1eabfa
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후처리
- 1온도cooling
- 2온도while heating
- 3온도under reflux for 4 hours
- 4세척The resulting mixture was washed with a saturated aqueous ammonium chloride solution and saturated brine
- 5농축concentrated under reduced pressure
- 6기타The residue was purified by silica gel column chromatography
실험 절차
The compound of Example B205 (800 μl, 0.3 mmol) was added to a solution of 1-chloropyrrolopyridine (19.4 mg, 0.127 mmol), which was synthesized from 2-chloro-3-aminopyridine according to the method of H07-165,708A, and dichloro(diphenylphosphinopropane)nickel (6.9 mg, 0.013 mmol) in tetrahydrofuran (1 ml) under ice-cooling, and the mixture was stirred while heating under reflux for 4 hours. After allowing the mixture to cool to room temperature, ethyl acetate was added thereto. The resulting mixture was washed with a saturated aqueous ammonium chloride solution and saturated brine, then concentrated under reduced pressure. The residue was purified by silica gel column chromatography to give the title compound (7.1 mg).