反応 #1071943
ord-0e1c8a71196d4753a61e5b592f8c8adb
溶媒
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1温度refluxed under N for 20 h
- 2その他was removed by distillation
- 3workup.DISSOLUTIONthe residue was redissolved in H2O
- 4その他was obtained This product
- 5ろ過was collected by filtration
- 6洗浄washed with cold H2O
- 7その他then crystallized from dilute MeOH
- 8その他to give colorless needles
実験手順
EtOH (30 mL) was added to 2,5-dicarbethoxy-3,4-dihydroxythiophene (1 g). A solution of NaOH (4.0 g) in H2O (20 mL) was added and refluxed under N for 20 h. Upon cooling to ambient temperature the EtOH was removed by distillation and the residue was redissolved in H2O then acidified with 15% HClaq when a white ppt was obtained This product was collected by filtration and washed with cold H2O then crystallized from dilute MeOH to give colorless needles.