反応 #171817
ord-f93db726695745e9b2a4f1d416c38efe
反応方程式
反応物
溶媒
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1その他was reacted in the microwave at 160° C. for 4 h
- 2その他The mixture was then partitioned between dichloromethane (30 mL) and water (20 mL)
- 3乾燥The organic layer was dried (MgSO4)
- 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.