Hydrochloric Acid → 2-Methylthiophene-3-carboxylic acid
反応式
[CH3:1][C:2]1[S:3][CH:4]=[CH:5][C:6]=1[C:7]([O:9]CC)=[O:8].[OH-].[Na+].Cl>C(O)C.O>[CH3:1][C:2]1[S:3][CH:4]=[CH:5][C:6]=1[C:7]([OH:9])=[O:8]参加物
6
実験手順
Ethyl 2-methyl-3-thiophenecarboxylate (3.42 g, 20.09 mmol; see step (ii) above) was dissolved in ethanol (5 mL) to which was added a solution of sodium hydroxide (3.2145 mg, 80.362 mmol) in water (10 mL). The reaction mixture was heated under reflux for 2 h. The volume was reduced to half under reduced pressure at 40° C. and the residue was cooled with ice water. Dilute HCl was added dropwise with stirring until pH 2. The white solid material was filtered off, washed with water and dried under reduced pressure at 50° C. to give the required material (2.1850 mg, 77% yield), m.p. 115-117° C., lit. m.p. 116-117° C. (see D. W. Knight, A. P. Nott J. Chem. Soc., Perkin Trans. 1 791-794 (1983)).
後処理
- temperatureThe reaction mixture was heated
- temperatureunder reflux for 2 h
- customwas reduced to half under reduced pressure at 40° C.
- filtrationThe white solid material was filtered off
- washwashed with water
- customdried under reduced pressure at 50° C.
出典と根拠
- ORDレコード
- ord-f49607a9e93249daaab070e2dcce2746
- 出典データセット
- uspto-grants-2010_04
- 特許番号
- US07700765B2
反応ノート
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