反应 #367460

反应方程式

4-Aminobutanoic acid

sodium methoxide

(5-chloro-2-hydroxy-3-methylphenyl)-(4-chlorophenyl)-methanone

ethanol

→

4-{[(5-Chloro-2-hydroxy-3-methylphenyl)-(4-chlorophenyl)-methylene]-amino}-butanoic acid

溶剂

methanol

反应条件

后处理

1. 1
   其他the resulting mixture is then evaporated to dryness
2. 2
   workup.ADDITIONEthanol (500 ml) is added to the residue
3. 3
   其他the mixture is then evaporated to dryness
4. 4
   workup.DISSOLUTIONThe residue is dissolved in 1 liter of water
5. 5
   workup.ADDITIONthe pH is acidified to pH 4 by the addition of citric acid
6. 6
   过滤The precipitate is filtered off
7. 7
   洗涤washed with water
8. 8
   workup.DISSOLUTIONdissolved in CH2Cl2
9. 9
   洗涤The organic solution is washed with water
10. 10
    干燥dried (MgSO4)
11. 11
    过滤filtered
12. 12
    其他the filtrate is evaporated
13. 13
    其他to give an oil, which
14. 14
    其他is crystallised once from petroleum ether
15. 15
    其他recrystallised twice from AcOEt

实验过程

4-Aminobutanoic acid (2.2 g; 0.0213 mol), sodium methoxide (1.16 g; 0.0213 mol) and (5-chloro-2-hydroxy-3-methylphenyl)-(4-chlorophenyl)-methanone (6 g; 0.0213 mol) are introduced into a mixture of 200 ml of ethanol and 400 ml of methanol, and the resulting mixture is then evaporated to dryness. Ethanol (500 ml) is added to the residue and the mixture is then evaporated to dryness. The latter operation is repeated 4 times. The residue is dissolved in 1 liter of water and the pH is acidified to pH 4 by the addition of citric acid. The precipitate is filtered off, washed with water and then dissolved in CH2Cl2. The organic solution is washed with water, dried (MgSO4) and filtered, and the filtrate is evaporated to give an oil, which is crystallised once from petroleum ether and recrystallised twice from AcOEt.

来源