Sulfuryl chloride → ethyl 3-chloro-2,4-dioxopentanoate
反応式
S(Cl)([Cl:4])(=O)=O.[O:6]=[C:7]([CH2:13][C:14](=[O:16])[CH3:15])[C:8]([O:10][CH2:11][CH3:12])=[O:9]>C(Cl)Cl>[Cl:4][CH:13]([C:14](=[O:16])[CH3:15])[C:7](=[O:6])[C:8]([O:10][CH2:11][CH3:12])=[O:9]参加物
4
実験手順
A solution of sulfuryl chloride (7.08 g, 52 mmol) in 15 mL of CH2Cl2 was added dropwise to a solution of ethyl 2,4-dioxovalerate (7.91 g, 40 mmol) in 125 ml of CH2Cl2 at room temperature. After three hours TLC analysis indicated that all of the starting material had been consumed. The reaction mixture was washed with H2O (2×100 mL), dried over anhydrous MgSO4, filtered and concentrated in vacuo to give 7.84 g (81% yield) of the desired product as and orange oil: 1H NMR (CDCl3) 67 14.4 (bs, 1H), 5.4 (s, 1H), 4.4-4.3 (m, 4H), 2.5 (s, 3H), 2.4 (s, 3H), 1.4-1.35 (s, 6H) for a 1:1 mixture of tautomers.
後処理
- customhad been consumed
- washThe reaction mixture was washed with H2O (2×100 mL)
- dry with materialdried over anhydrous MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-f9a4d8d0e71d48f89f19c091c61bca21
- 出典データセット
- uspto-grants-2000_08
- 特許番号
- US06096898
反応ノート
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