反応 #1071943

ord-0e1c8a71196d4753a61e5b592f8c8adb

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度refluxed under N for 20 h
  2. 2
    その他was removed by distillation
  3. 3
    workup.DISSOLUTIONthe residue was redissolved in H2O
  4. 4
    その他was obtained This product
  5. 5
    ろ過was collected by filtration
  6. 6
    洗浄washed with cold H2O
  7. 7
    その他then crystallized from dilute MeOH
  8. 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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06869729B1uspto-grants-2005_03