반응식
[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]=1참가 물질
8
반응물 4
생성물 1
시약·촉매·용매 3
반응 조건
- 온도
- 120 °C
실험 절차
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.
후처리
- 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.
출처 및 근거
- ORD 기록
- ord-33f5c2c61cec497c9cae12b9bafc104f
- 출처 데이터셋
- uspto-grants-1998_03
- 특허 번호
- US05726315
연결된 노트
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