反応 #824110

反応方程式

NaOH

diethyl 2-(4-amino-3-chloro-5-trifluoromethyl-benzyl)-2-{2-oxo-2-[4-(2-oxo-1,4-dihydro-2H-quinazolin-3-yl)-piperidin-1-yl]-ethyl}-malonate

→

2-(4-amino-3-chloro-5-trifluoromethyl-benzyl)-4-oxo-4-[4-(2-oxo-1,4-dihydro-2H-quinazolin-3-yl)-piperidin-1-yl]-butanoic acid

溶媒

water

EtOH

反応条件

後処理

1. 1
   温度the mixture was refluxed for 4 h
2. 2
   その他EtOH was evaporated off i
3. 3
   その他was acidified to pH 1 with conc. HCl and 1 hour at RT
4. 4
   その他The precipitate formed
5. 5
   ろ過was filtered off
6. 6
   洗浄washed with water
7. 7
   その他dried i

実験手順

3.13 g (78.25 mmol) of NaOH, dissolved in 300 mL water, were added to a solution of 10.00 g (15.65 mmol) of diethyl 2-(4-amino-3-chloro-5-trifluoromethyl-benzyl)-2-{2-oxo-2-[4-(2-oxo-1,4-dihydro-2H-quinazolin-3-yl)-piperidin-1-yl]-ethyl}-malonate in 600 mL EtOH and the mixture was refluxed for 4 h. EtOH was evaporated off i. vac., the reaction mixture was acidified to pH 1 with conc. HCl and 1 hour at RT. The precipitate formed was filtered off, washed with water and dried i. vac.

出典