Methanol → Methyl 4-hydroxythiophene-2-carboxylate
反応式
S(Cl)(Cl)=O.[OH:5][C:6]1[CH:7]=[C:8]([C:11]([OH:13])=[O:12])[S:9][CH:10]=1.[CH3:14]O>>[OH:5][C:6]1[CH:7]=[C:8]([C:11]([O:13][CH3:14])=[O:12])[S:9][CH:10]=1参加物
4
実験手順
Thionyl chloride (1.6 ml) was added dropwise to a methanol solution (20 ml) of 4-hydroxythiophene-2-carboxylic acid (1.1 g, 7.6 mmol) under ice cooling. The solution mixture was refluxed with heating for 5 hours. The reaction solution was cooled to room temperature, poured into ice water and extracted with ethyl acetate. The extraction solution with ethyl acetate was dried over magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=4:1) and concentrated/dried under reduced pressure to obtain methyl 4-hydroxythiophene-2-carboxylate (0.7 g) as white powder.
後処理
- temperatureThe solution mixture was refluxed
- temperaturewith heating for 5 hours
- extractionextracted with ethyl acetate
- dry with materialThe extraction solution with ethyl acetate was dried over magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=4:1)
- customconcentrated/dried under reduced pressure
出典と根拠
- ORDレコード
- ord-ced317196d414c2fb17a3d74f0497f09
- 出典データセット
- uspto-grants-2013_12
- 特許番号
- US08598162B2
反応ノート
読み込み中…