反応式
C1(S[CH:8]([C:12]2[S:13][CH:14]=[CH:15][CH:16]=2)[C:9]([OH:11])=[O:10])C=CC=CC=1>C(O)(=O)C.[Zn]>[S:13]1[CH:14]=[CH:15][CH:16]=[C:12]1[CH2:8][C:9]([OH:11])=[O:10]参加物
実験手順
α-Phenylthio-2-thiopheneacetic acid (890 mg, 3.56 mmol) was dissolved in acetic acid (6 ml), then zinc dust (350 mg, 5.4 mmol) was added and the mixture was heated under reflux with vigorous stirring. After 30 min., zinc dust (350 mg, 5.4 mmol) was added again, and the mixture was heated under reflux for another 4 hr. with stirring, then cooled to room temperature, and most of the solvent was removed by distillation. Water and ethyl acetate were added and the precipitate was filtered off by the use of celite, and the layers of the filtrate were separated. The organic layer was washed with an aqueous solution of sodium chloride and dried with anhydrous magnesium sulfate. After filtration, the solution was concentrated under a reduced pressure and the crystals thus obtained were further recrystallized from ethyl acetate: n-hexane to give 2-thiopheneacetic acid (430 mg) melting at 62° C. (literature value: 62°-65° C.).
後処理
- temperaturethe mixture was heated
- temperatureunder reflux with vigorous stirring
- temperaturethe mixture was heated
- temperatureunder reflux for another 4 hr
- custommost of the solvent was removed by distillation
- additionWater and ethyl acetate were added
- filtrationthe precipitate was filtered off by the use of celite
- customthe layers of the filtrate were separated
- washThe organic layer was washed with an aqueous solution of sodium chloride
- dry with materialdried with anhydrous magnesium sulfate
- filtrationAfter filtration
- concentrationthe solution was concentrated under a reduced pressure
- customthe crystals thus obtained
- customwere further recrystallized from ethyl acetate
出典と根拠
- ORDレコード
- ord-e87aeb7cbdaa4eca9de86254627b734a
- 出典データセット
- uspto-grants-1980_09
- 特許番号
- US04221915
関連ノート
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