反応 #715229

ord-561200e112464d54ab54bba843556302

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他was reacted in the microwave at 160° C. for 4 h
  2. 2
    その他The mixture was then partitioned between dichloromethane (30 mL) and water (20 mL)
  3. 3
    乾燥The organic layer was dried (MgSO4)
  4. 4
    その他purified on silica

実験手順

A mixture of 9-bromo-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulene-2-carboxylic acid ethyl ester (500 mg), potassium ferrocyanide (dried, 104 mg), copper (I) iodide (27 mg) and 1-butylimidazole (0.37 mL) in toluene (3 mL) was reacted in the microwave at 160° C. for 4 h. The mixture was then partitioned between dichloromethane (30 mL) and water (20 mL). The organic layer was dried (MgSO4), reduced in vacuo and purified on silica to give 9-cyano-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulene-2-carboxylic acid ethyl ester.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09309265B2uspto-grants-2016_04