Piperazine → HCID 20463845、化合物
反応式
[Cl:1][C:2]1[C:7]([I:8])=[CH:6][CH:5]=[CH:4][N:3]=1.[NH:9]1[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1>CCCCO>[ClH:1].[ClH:1].[I:8][C:7]1[C:2]([N:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)=[N:3][CH:4]=[CH:5][CH:6]=1参加物
4
実験手順
A solution of 2-chloro-3-iodopyridine (2.39 g, 10 mmol) and piperazine (8.61 g, 100 mmol) in n-BuOH, 100 mL, was stirred at reflux under N2 for 18 h. After removing most of the n-BuOH under reduced pressure, the residue was partitioned between toluene and 10% NaOH. The toluene layer was washed further with water, dried (Na2SO4), filtered and concentrated to an oil. The pyridinylpiperazine was purified by recrystallization of the dihydrochloride salt from methanol-ethanol-ethylacetate, m.p. 185°-189° C. (dec.).
後処理
- temperatureat reflux under N2 for 18 h
- customAfter removing most of the n-BuOH under reduced pressure
- customthe residue was partitioned between toluene and 10% NaOH
- washThe toluene layer was washed further with water
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated to an oil
- customThe pyridinylpiperazine was purified by recrystallization of the dihydrochloride salt from methanol-ethanol-ethylacetate, m.p. 185°-189° C. (dec.)
出典と根拠
- ORDレコード
- ord-00935eeeacfe4bd7ae4b13aaeafd3b75
- 出典データセット
- uspto-grants-1984_04
- 特許番号
- US04442103
反応ノート
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