反応 #55742

反応方程式

pyridine

2-ethoxy-5-chloro-benzoyl chloride

acetone

4-(2-aminoethyl)-benzoic acid methyl ester-hydrochloride

acetone

→

benzoic acid methyl ester

溶媒

dioxane

反応条件

後処理

1. 1
   温度the whole was heated for 2 hours
2. 2
   温度under reflux
3. 3
   温度After cooling
4. 4
   濃縮the mixture was concentrated under reduced pressure
5. 5
   ろ過filtered with suction
6. 6
   workup.STIRRINGstirred with dilute hydrochloric acid and with a NaHCO3 solution
7. 7
   ろ過the resulting product was again filtered off with suction
8. 8
   その他recrystallized from ethanol

実験手順

10.5 g of 4-(2-aminoethyl)-benzoic acid methyl ester-hydrochloride were suspended in 40 ml of dioxane and 20 ml of acetone and the suspension was combined with 8 ml of pyridine. To this suspension, a solution of 10 g of 2-ethoxy-5-chloro-benzoyl chloride in a small amount of acetone was added dropwise, while stirring, and the whole was heated for 2 hours under reflux. After cooling, the mixture was concentrated under reduced pressure, combined with ice-water, filtered with suction, stirred with dilute hydrochloric acid and with a NaHCO3 solution and the resulting product was again filtered off with suction and recrystallized from ethanol. The 4-(2-<2-ethoxy-5-chloro-benzamido>-ethyl)-benzoic acid methyl ester obtained was found to melt at 110° C.

出典