反応式
[F:1][C:2]([F:15])([F:14])[C:3]1[CH:4]=[C:5]([CH2:9][C:10]([O:12][CH3:13])=[O:11])[CH:6]=[CH:7][CH:8]=1.[CH:16](OC)=[O:17].[Na].Cl>C(OCC)C>[OH:17][CH:16]=[C:9]([C:5]1[CH:4]=[C:3]([C:2]([F:14])([F:15])[F:1])[CH:8]=[CH:7][CH:6]=1)[C:10]([O:12][CH3:13])=[O:11]参加物
6
実験手順
(aa) 26.2 g of methyl 3-trifluoromethylphenylacetate were dissolved in 100 ml of diethyl ether and, after the addition of 8.2 ml of methyl formate, treated with 2.76 g of sodium. The mixture was stirred at room temperature until the reaction was completed and treated with 1N hydrochloric acid while cooling. The organic phase was separated and the aqueous phase was extracted twice with ether. The combined organic phases were washed with saturated sodium chloride solution, dried over sodium sulfate, filtered and evaporated. Distillation yielded methyl 3-hydroxy-2-(α,α,α-trifluoro-m-tolyl)acrylate as a colorless oil of b.p. 59°-62°/0.2 mm.
後処理
- temperaturewhile cooling
- customThe organic phase was separated
- extractionthe aqueous phase was extracted twice with ether
- washThe combined organic phases were washed with saturated sodium chloride solution
- dry with materialdried over sodium sulfate
- filtrationfiltered
- customevaporated
- distillationDistillation
出典と根拠
- ORDレコード
- ord-0a8397fc083c47c09bc3122845ef585d
- 出典データセット
- uspto-grants-1989_12
- 特許番号
- US04889848
関連ノート
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