反応式
[H-].[Na+].[CH3:3][O:4][C:5]1[CH:10]=[C:9]([O:11][CH3:12])[N:8]=[C:7]([O:13][C:14]2[CH:22]=[CH:21][CH:20]=[CH:19][C:15]=2[C:16]([OH:18])=[O:17])[N:6]=1.Br[CH2:24][CH2:25][CH:26]1[O:30][CH2:29][CH2:28][O:27]1.Cl>C(Cl)(Cl)Cl.CN(C)C=O>[CH3:12][O:11][C:9]1[CH:10]=[C:5]([O:4][CH3:3])[N:6]=[C:7]([O:13][C:14]2[CH:22]=[CH:21][CH:20]=[CH:19][C:15]=2[C:16]([O:18][CH2:24][CH2:25][CH:26]2[O:30][CH2:29][CH2:28][O:27]2)=[O:17])[N:8]=1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
10 Milliliters of N,N-dimethylformamide in which 0.22 g of 60% sodium hydride in oil has been suspended was mixed with 5 ml of N,N-dimethylformamide solution of 1.38 g of 2-(4,6-dimethoxypyrimidin-2-yl)oxy benzoic acid. After stirring the mixture at room temperature for 30 minutes, 10 ml of N,N-dimethylformamide solution of 1.81 g of 2-(2-bromoethyl)-1,3-dioxolane was added thereto. The resulting solution was stirred at 100° to 110° C. for 2 hours. The reaction solution was allowed to cool, poured into diluted hydrochloric acid, and extracted with ethyl acetate. The organic layer separated from the aqueous layer was washed with saturated sodium chloride solution and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the residue obtained was subjected to silica gel column chromatography (mfd. by Merck & Co., Inc., solvent: chloroform) to obtain 1.20 g of 2-(1,3-dioxolan-2-yl)ethyl 2-(4,6-dimethoxypyrimidin-2-yl)oxybenzoate [present compound (V-2)].
後処理
- stirringThe resulting solution was stirred at 100° to 110° C. for 2 hours
- temperatureto cool
- extractionextracted with ethyl acetate
- customThe organic layer separated from the aqueous layer
- washwas washed with saturated sodium chloride solution
- dry with materialdried over anhydrous magnesium sulfate
- customThe solvent was removed under reduced pressure
- customthe residue obtained
出典と根拠
- ORDレコード
- ord-57289cd2ff5e490b8cb79b1e767d633f
- 出典データセット
- uspto-grants-1994_03
- 特許番号
- US05298632
関連ノート
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