反応 #1352201

反応方程式

3,4-(methylenedioxy)toluene

DMF

phosphorus oxychloride

→

title compound

収率 11.0%

2-Methyl-4,5-(methylenedioxy)benzaldehyde

収率 11.0%

溶媒

反応条件

後処理

1. 1
   温度The solution was heated to 110° C. upon which it
2. 2
   温度1.5 hours later the thick dark brown mixture was cooled to ambient temperature
3. 3
   抽出extracted with ether (100 ml)
4. 4
   乾燥The organic layer was dried (MgSO4)
5. 5
   ろ過filtered
6. 6
   濃縮concentrated

実験手順

To DMF (6.5 ml, 83 mmoles) at 0° C. was added phosphorus oxychloride (3.9 ml, 42 mmoles). The solution was stirred 15 minutes at 0° C. followed by the addition of 3,4-(methylenedioxy)toluene (1.0 ml, 8.3 mmoles). The solution was heated to 110° C. upon which it became dark brown. 1.5 hours later the thick dark brown mixture was cooled to ambient temperature then added to ice (100 ml), and extracted with ether (100 ml). The organic layer was dried (MgSO4), filtered and concentrated. Flash chromatography (5% EtOAc/hexanes) provided 0.15 g (11%) of the title compound as a colorless oil.

出典