反応式
[Cl:1][C:2]1[S:6][C:5]([C:7]([OH:9])=[O:8])=[C:4]([Si:10]([CH3:13])([CH3:12])[CH3:11])[CH:3]=1.S(Cl)([Cl:16])=O.Cl.[CH:19]([NH:22][OH:23])([CH3:21])[CH3:20].C([O-])(O)=O.[Na+]>C(Cl)Cl.O>[Cl:1][C:2]1[S:6][C:5]([C:7]([Cl:16])=[O:8])=[C:4]([Si:10]([CH3:13])([CH3:12])[CH3:11])[CH:3]=1.[Cl:1][C:2]1[S:6][C:5]([C:7]([N:22]([OH:23])[CH:19]([CH3:21])[CH3:20])=[O:9])=[C:4]([Si:10]([CH3:13])([CH3:12])[CH3:11])[CH:3]=1参加物
8
反応物 4
生成物 2
試薬・触媒・溶媒 2
実験手順
5-Chloro-3-(trimethylsilyl)-2-thiophenecarboxylic acid chloride was prepared by the reaction of 1 g 5-chloro-3-(trimethylsilyl)-2-thiophenecarboxylic acid (prepared as in Example 263) and 6 mL thionyl chloride, using the procedure of step a in Example 248. This product was dissolved in CH2Cl2 at 0° C. and added to a mixture of N-isopropylhydroxylamine hydrochloride (0.55 g, 5 mmol) and 4 g NaHCO3 in 20 mL CH2Cl2 and 20 mL water. The resulting reaction mixture was stirred at RT for additional 3 h. The organic layer was separated, washed with brine, dried and concentrated. The residue was purified by flash chromatography with 8% ethyl acetate/hexane to give 80 mg of the title compound. m.p. 146-150° C.
後処理
- customThe resulting reaction mixture
- customThe organic layer was separated
- washwashed with brine
- customdried
- concentrationconcentrated
- customThe residue was purified by flash chromatography with 8% ethyl acetate/hexane
出典と根拠
- ORDレコード
- ord-c37b8ad86da54ac585df07c537d76f95
- 出典データセット
- uspto-grants-2000_10
- 特許番号
- US06133252
関連ノート
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