反応式
[OH:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:10]=1[C:9](=[S:11])[O:8][CH:7]2[CH3:12].[H-].[Na+].[H][H].Cl[C:18]1[N:23]=[C:22]([O:24][CH3:25])[N:21]=[C:20]([O:26][CH3:27])[N:19]=1>CN(C)C=O>[CH3:27][O:26][C:20]1[N:21]=[C:22]([O:24][CH3:25])[N:23]=[C:18]([O:1][C:2]2[CH:3]=[CH:4][CH:5]=[C:6]3[C:10]=2[C:9](=[S:11])[O:8][CH:7]3[CH3:12])[N:19]=1参加物
実験手順
1.0 g of 7-hydroxy-3-methyl-isobenzofuran-1(3H)-thione is introduced into a suspension of 0.15 g of sodium hydride in absolute dimethylformamide and, when the evolution of hydrogen has ceased, 1.0 g of 2-chloro-4,6-dimethoxy-1,3,5-triazine is added thereto. The reaction mixture is subsequently stirred at room temperature for 5 hours, ice-water is then added and the whole is extracted with ethyl acetate and washed with sodium chloride solution. The crude product, having been concentrated by evaporation, is purified by chromatography (eluant: 45% ethyl acetate in n-hexane) and recrystallised from acetone/n-hexane to yield 7-[(4,6-dimethoxy-1,3,5-triazin-2-yl)oxy]-3-methyl-isobenzofuran-1(3H)-thione in the form of yellow crysals, m.p. 177°-178° C.; IR spectrum (CHCl3): 1590, 1560, 1366, 1304, 1140 cm-1 ; 1H-NMR (CDCl3): 5.81 ppm (q, 1H), 1.73 ppm (d, 3H).
後処理
- extractionthe whole is extracted with ethyl acetate
- washwashed with sodium chloride solution
- concentrationThe crude product, having been concentrated by evaporation
- customis purified by chromatography (eluant: 45% ethyl acetate in n-hexane)
- customrecrystallised from acetone/n-hexane
出典と根拠
- ORDレコード
- ord-6bb2c1b7ef404f27a231b4a9a16bd962
- 出典データセット
- uspto-grants-1995_06
- 特許番号
- US05428002
関連ノート
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