反応式
[CH2:1]([O:3][CH:4]([CH2:10][C:11]1[CH:16]=[CH:15][C:14]([OH:17])=[C:13]([CH3:18])[CH:12]=1)[C:5]([O:7][CH2:8][CH3:9])=[O:6])[CH3:2].[CH3:19][S:20]([O:23][C:24]1[CH:29]=[CH:28][C:27]([CH2:30][CH2:31]OS(C)(=O)=O)=[CH:26][CH:25]=1)(=[O:22])=[O:21].C(=O)([O-])[O-].[K+].[K+]>CC(=O)CC>[CH2:1]([O:3][CH:4]([CH2:10][C:11]1[CH:16]=[CH:15][C:14]([O:17][CH2:31][CH2:30][C:27]2[CH:26]=[CH:25][C:24]([O:23][S:20]([CH3:19])(=[O:21])=[O:22])=[CH:29][CH:28]=2)=[C:13]([CH3:18])[CH:12]=1)[C:5]([O:7][CH2:8][CH3:9])=[O:6])[CH3:2]参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
Ethyl 2-ethoxy-3-(4-hydroxy-3-methylphenyl)propanoate (0.27 g, 1.05 mmole) and 4-{2-[(methylsulfonyl)oxy]ethyl}phenyl methanesulfonate (0.62 g, 2.11 mmole) were dissolved in 2-butanone (10 ml). Polyethyleneglycol 400 (0.20 g) and anhydrous potassium carbonate (0.22 g, 1.58 mmole) were added the mixture. After stirring at reflux for 16 hours it was checked with using HPLC whether all the starting material was consumed. The mixture was washed with water dried with magnesium sulfate and evaporated. Purification of the crude product with preparative HPLC (Kromasil C8, 7 μm, 50×250 mm) using actonitrile(60-80%) in ammonium acetate buffer (pH 7) as mobile phase gave 0.28 g (54% yield) of the desired product.
後処理
- temperatureat reflux for 16 hours it
- customwas consumed
- washThe mixture was washed with water
- dry with materialdried with magnesium sulfate
- customevaporated
- customPurification of the crude product with preparative HPLC (Kromasil C8, 7 μm, 50×250 mm)
出典と根拠
- ORDレコード
- ord-02697ed671954d6796654a028d818447
- 出典データセット
- uspto-grants-2004_06
- 特許番号
- US06750252B2
関連ノート
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