反応式
[OH:1][C:2]1[C:3](I)=[N:4][C:5]([CH2:8][OH:9])=[CH:6][CH:7]=1.C([O-])(=O)C.[K+].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[C:35]([O:39][CH2:40][CH3:41])(=[O:38])[CH:36]=[CH2:37]>CN(C=O)C.O.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[OH:1][C:2]1[C:3]([CH:37]=[CH:36][C:35]([O:39][CH2:40][CH3:41])=[O:38])=[N:4][C:5]([CH2:8][OH:9])=[CH:6][CH:7]=1参加物
8
反応物 4
生成物 1
試薬・触媒・溶媒 3
反応条件
- 温度
- 120 °C
実験手順
To a solution of 3-hydroxy-6-hydroxymethyl-2-iodopyridine (708 mg, 2.82 mmol) in DMF (5.7 ml) and water (0.3 ml) were added potassium acetate (0.74 g, 7.5 mmol), triphenylphosphine (63 mg, 0.24 mmol), ethyl acrylate (0.98 ml, 0.90 g, 9.0 mmol) and palladium acetate (27 mg, 0.12 mmol). The mixture was placed under nitrogen and stirred and heated at 120° C. for 5 h. The mix was cooled and poured into water (50 ml). The product was extracted into ethyl acetate (3×20 ml) and the combined extracts were washed with water (2×15 ml) with brine (15 ml), dried and evaporated. The etude product was purified by passage in ethyl acetate through a pad of silica, yielding after evaporation a yellow solid (295 g, 47%). mp (B.HCl) 199°-203° C.
後処理
- temperatureThe mix was cooled
- extractionThe product was extracted into ethyl acetate (3×20 ml)
- washthe combined extracts were washed with water (2×15 ml) with brine (15 ml)
- customdried
- customevaporated
- customThe etude product was purified by passage in ethyl acetate through a pad of silica
- customyielding
- customafter evaporation a yellow solid (295 g, 47%)
- custommp (B.HCl) 199°-203° C.
出典と根拠
- ORDレコード
- ord-33f5c2c61cec497c9cae12b9bafc104f
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05726315
関連ノート
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