반응 #11452
ord-0ffe6b5de4da45809dc6e19496796e1f
반응 방정식
반응 조건
후처리
- 1농축it was concentrated under reduced pressure
- 2기타The residue was partitioned between ethyl acetate and water
- 3기타The layers were separated
- 4추출the aqueous layer was extracted with ethyl acetate
- 5세척washed with brine
- 6건조dried over sodium sulfate
- 7농축concentrated under reduced pressure
- 8기타to provide an orange oil
- 9기타The oil was purified by flash chromatography (400 mL silica gel eluting initially with 10% ethyl acetate in hexane
실험 절차
A solution of 4-(2-aminoethyl)-1-benzylpiperidine (9.88 g, 45.2 mmol) in N,N-dimethylformamide was added dropwise to a solution of 2,4-dichloro-5,6-dimethyl-3-nitropyridine (10.00 g, 45.2 mmol) and triethylamine (12.6 mL, 90.5 mmol) in N,N-dimethylformamide (320 mL). The reaction mixture was allowed to stir at ambient temperature for about 20 hours and then it was concentrated under reduced pressure. The residue was partitioned between ethyl acetate and water. The layers were separated and the aqueous layer was extracted with ethyl acetate. The organics were combined, washed with brine, dried over sodium sulfate and then concentrated under reduced pressure to provide an orange oil. The oil was purified by flash chromatography (400 mL silica gel eluting initially with 10% ethyl acetate in hexane, then with 15% ethyl acetate in hexane and finally with 40% ethyl acetate in hexane) to provide 11.00 g of N-[2-(1-benzylpiperidin-4-yl)ethyl]-2-chloro-5,6-dimethyl-3-nitropyridin-4-amine.