反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5](Br)=[CH:4][N:3]=1.[C:9]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])(=[O:12])[CH:10]=[CH2:11].C(N(CC)CC)C.C1(C)C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C>CC#N.CC([O-])=O.CC([O-])=O.[Pd+2]>[C:14]([O:13][C:9](=[O:12])[CH:10]=[CH:11][C:5]1[CH:4]=[N:3][C:2]([NH2:1])=[CH:7][CH:6]=1)([CH3:17])([CH3:16])[CH3:15]参加物
7
反応条件
- 温度
- 110 °C
実験手順
A mixture of 2-amino-5-bromopyridine 10-1 (10 g, 58 mmol), tert-butyl acrylate (50 mL, 344 mmol), triethylamine (50 mL, 359 mmol), tri-o-tolylphosphine (3.0 g, 9.8 mmol) and Pd(OAc)2 (1.0 g, 4.5 mmol) in 150 mL CH3CN was purged with argon for 5 min and subsequently refluxed at 110° C. for 20 hr. The mixture was then cooled and concentrated. The residue was purified using silica gel flash chromatography (EtOAc/hexanes 1:1) to afford the desired product 10-2 as a solid.
後処理
- customwas purged with argon for 5 min
- temperatureThe mixture was then cooled
- concentrationconcentrated
- customThe residue was purified
出典と根拠
- ORDレコード
- ord-2eabb9cffcb24e7ab6ee6ae981a3b4b3
- 出典データセット
- uspto-grants-2001_07
- 特許番号
- US06268378B1
関連ノート
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