反応 #60744

反応方程式

water

diethylamine

2-hydroxy-4′-methoxyacetophenone

malononitrile

→

intermediate

収率 87.0%

2-Amino-3-cyano-4-(4-methoxyphenyl)furan

収率 87.0%

溶媒

DMF

反応条件

後処理

1. 1
   ろ過The precipitate was filtrated
2. 2
   洗浄washed with water
3. 3
   その他dried under reduced pressure

実験手順

To a cooled solution of 2-hydroxy-4′-methoxyacetophenone (379 mg, 2.28 mmol) in DMF (0.75 ml) was added malononitrile (166 mg, 2.51 mmol) followed by diethylamine (0.1 ml, 0.97 mmol). The mixture was stirred at room temperature for 2 hours, and then poured into large amount of cold water. The precipitate was filtrated, washed with water, and dried under reduced pressure to give the intermediate of Example 1(A) (424 mg, 87%) as a brown solid. 1H NMR (400 MHz, CDCl3) ppm 3.83 (s, 3H), 4.73 (brs, 2H), 6.93 (m, 2H), 6.94 (s, 1H), 7.49 (m, 2H). LC/MS: m/z 215 (M+1)+.

出典