反応式
[CH3:1][O:2][C:3](=[O:28])[CH2:4][CH2:5][C:6]1[NH:7][C:8](I)([O:12][CH2:13][CH2:14][CH2:15][CH2:16]/[CH:17]=[CH:18]/[C:19]2[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][CH:20]=2)[CH:9]=[CH:10][CH:11]=1.[CH2:29]([O:31]C=C[Sn](CCCC)(CCCC)CCCC)[CH3:30]>C1(C)C=CC=CC=1>[CH3:1][O:2][C:3](=[O:28])[CH2:4][CH2:5][C:6]1[NH:7][C:8]([C:29](=[O:31])[CH3:30])([O:12][CH2:13][CH2:14][CH2:15][CH2:16]/[CH:17]=[CH:18]/[C:19]2[CH:24]=[CH:23][C:22]([O:25][CH3:26])=[CH:21][CH:20]=2)[CH:9]=[CH:10][CH:11]=1参加物
4
反応条件
- 温度
- 110 °C
実験手順
A solution of 495 mg of 3-{6-iodo-3-[6-(4-methoxyphenyl-(5E)-5-hexenyloxy]-2-pyridyl}-propionic acid methyl ester and 397 mg of ethoxyvinyltributyltin in 2 ml of toluene is mixed with 30 mg of bis-triphenylphosphine-palladium(II) chloride and heated for six hours with stirring to 110° C. The reaction mixture is filtered on diatomaceous earth, the filter residue is washed with diethyl ether, the filtrate is mixed with 1.5 ml of 2n hydrochloric acid and stirred for 4 hours at room temperature. The organic phase is separated, dried with sodium sulfate and concentrated by evaporation. 95 mg of 3-{6-acetyl-3-[6-(4-methoxyphenyl-(5E)-5-hexenyloxy]-2-pyridyl}-propionic acid methyl ester is obtained as oil.
後処理
- temperatureheated for six hours
- filtrationThe reaction mixture is filtered on diatomaceous earth
- washthe filter residue is washed with diethyl ether
- additionthe filtrate is mixed with 1.5 ml of 2n hydrochloric acid
- stirringstirred for 4 hours at room temperature
- customThe organic phase is separated
- dry with materialdried with sodium sulfate
- concentrationconcentrated by evaporation
出典と根拠
- ORDレコード
- ord-5374a5b7c4d54206b10cb491f614f631
- 出典データセット
- uspto-grants-1997_04
- 特許番号
- US05624943
関連ノート
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