Triethylamine → 6-Bromo-N-cyclobutylpyridazin-3-amine
反応式
[Br:1][C:2]1[N:3]=[N:4][C:5](Br)=[CH:6][CH:7]=1.[CH:9]1([NH2:13])[CH2:12][CH2:11][CH2:10]1.CCN(CC)CC>O1CCOCC1>[Br:1][C:2]1[N:3]=[N:4][C:5]([NH:13][CH:9]2[CH2:12][CH2:11][CH2:10]2)=[CH:6][CH:7]=1参加物
5
実験手順
Into a solution of 3,6-dibromopyridazine (1.19 g, 5 mmol) in dioxane (5 mL) was added cyclobutylamine (0.39 g, 5.5 mmol), and Et3N (0.60 g, 6 mmol). The reaction was microwave at 90° C., 150 W for 0.45 h. The reaction was monitored by TLC and the crude product was purified by silica gel chromatography (eluent: 30% Ethyl acetate in n-hexane), to give the desired product (0.63 g, 55.3%). 1H NMR (300 MHz, CDCl3) δ: 7.25-7.28 (1H, d, J=9.0 Hz), 6.49-6.52 (1H, d, J=9.0 Hz), 5.27 (1H, s), 4.16-4.24 (1H, m), 2.40-4.49 (2H, m), 1.87-1.95 (2H, m), 1.75-1.84 (2H, m).
後処理
- customat 90° C.
- customthe crude product was purified by silica gel chromatography (eluent: 30% Ethyl acetate in n-hexane)
出典と根拠
- ORDレコード
- ord-bee6f9bffa35466797c4f98fedf30f34
- 出典データセット
- uspto-grants-2014_10
- 特許番号
- US08859553B2
反応ノート
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