反応 #1885019

反応方程式

iso-propyl 4-acetoxybut-2-ynecarboxylate

1-(6-chloropyridin-3-yl)-N-methylmethanamine

→

iso-Propyl 4-acetoxy-3-[(6-chloropyrid-3-ylmethyl)amino]but-2-enecarboxylate

溶媒

THF

tetrahydrofuran

反応条件

後処理

1. 1
   濃縮concentrated under reduced pressure
2. 2
   洗浄washed successively with dilute aqueous sulphuric acid and sodium hydrogencarbonate solution
3. 3
   乾燥After drying over magnesium sulphate
4. 4
   濃縮concentrating the organic phase under reduced pressure, 120 mg (50% of theory) of iso-propyl 4-acetoxy-3-[(4-chlorobenzyl)(methyl)amino]but-2-enecarboxylate
5. 5
   その他are obtained

実験手順

To an initial charge of 124 mg (0.672 mmol) of iso-propyl 4-acetoxybut-2-ynecarboxylate in 5 ml of anhydrous tetrahydrofuran (THF) are added dropwise 116 mg (0.739 mmol) of 1-(6-chloropyridin-3-yl)-N-methylmethanamine, dissolved in 1 ml of anhydrous THF, at room temperature. The reaction mixture is stirred at room temperature for 16 h and concentrated under reduced pressure. Subsequently, the residue is taken up with toluene and washed successively with dilute aqueous sulphuric acid and sodium hydrogencarbonate solution. After drying over magnesium sulphate and concentrating the organic phase under reduced pressure, 120 mg (50% of theory) of iso-propyl 4-acetoxy-3-[(4-chlorobenzyl)(methyl)amino]but-2-enecarboxylate are obtained.

出典