Triethylamine → 3-bromo-7-chloro-6,7-dihydro-5H-cyclopenta[b]pyridine
반응식
[Br:1][C:2]1[CH:3]=[N+:4]([O-])[C:5]2[CH2:6][CH2:7][CH2:8][C:9]=2[CH:10]=1.O=P(Cl)(Cl)[Cl:14].C(N(CC)CC)C>C(Cl)Cl>[Br:1][C:2]1[CH:3]=[N:4][C:5]2[CH:6]([Cl:14])[CH2:7][CH2:8][C:9]=2[CH:10]=1참가 물질
5
실험 절차
To a solution of 3-bromo-6,7-dihydro-5H-[1]pyrindine N-Oxide (250 mg, 1.17 mM) in 3 mL of CH2Cl2 at room temperature was added POCl3 (0.131 mL, 1.4 mM) and triethylamine (0.202 mL, 1.4 mM). The reaction was stirred at room temperature for 2 hours then was extracted from saturated NaHCO3 solution into ethyl acetate, washed with saturated NaCl, dried over MgSO4, filtered, and concentrated to dryness. The product was used crude in the next step. 1H NMR (CDCl3): d 8.60 (s, 1 H), 7.80 (s, 1 H), 5.40 (d, 1 H), 3.00 (m, 2 H), 2.20 (m, 2 H)
후처리
- extractionthen was extracted from saturated NaHCO3 solution into ethyl acetate
- washwashed with saturated NaCl
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated to dryness
출처 및 근거
- ORD 기록
- ord-808d67f9156c4dc2916c1831155253bd
- 출처 데이터셋
- uspto-grants-1994_08
- 특허 번호
- US05338740
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