반응 #1885019

반응 방정식

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

용매

THF

tetrahydrofuran

반응 조건

후처리

1. 1
   농축concentrated under reduced pressure
2. 2
   세척washed successively with dilute aqueous sulphuric acid and sodium hydrogencarbonate solution
3. 3
   건조After drying over magnesium sulphate
4. 4
   농축concentrating 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
   기타are obtained

실험 절차

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.

출처