反応 #82924

反応方程式

6-(4-morpholinyl)-3-[3-(trifluoromethyl)phenyl]-1,5(6H)-pyridazindicarboxylic acid, diethyl ester

water

→

6-[3-(trifluoromethyl)phenyl]-4-pyridazinecarboxylic acid ethyl ester

収率 47.0%

溶媒

DMF

反応条件

後処理

1. 1
   抽出extracted 3×100 mL with ethyl acetate
2. 2
   乾燥The organic layer was dried (MgSO4)
3. 3
   ろ過filtered through silica gel
4. 4
   その他evaporated in vacuo
5. 5
   その他to give a crude solid which
6. 6
   その他was recrystallized from cyclohexane/ethyl acetate

実験手順

6-(4-morpholinyl)-3-[3-(trifluoromethyl)phenyl]-1,5(6H)-pyridazindicarboxylic acid, diethyl ester (10.73 g, 0.024 mole) was refluxed in DMF (150 mL) for 30 min. The mixture was poured into water and extracted 3×100 mL with ethyl acetate. The organic layer was dried (MgSO4), filtered through silica gel, and evaporated in vacuo to give a crude solid which was recrystallized from cyclohexane/ethyl acetate to give 6-[3-(trifluoromethyl)phenyl]-4-pyridazinecarboxylic acid ethyl ester (3.34 g, 47% yield, Compound No. 1) as a brown solid.

出典