反応 #59053

反応方程式

hydrochloric acid

sodium hydroxide

ethyl 4′-(2-[(1S,2R)-2-hydroxy-2-(4-hydroxyphenyl)-1-methylethylamino]ethoxy)biphenyl-4-carboxylate

ethanol

sodium hydroxide

→

title compound

4′-{2-[(1S,2R)-2-Hydroxy-2-(4-hydroxyphenyl)-1-methylethyl-amino]ethoxy}biphenyl-4-carboxylic acid

溶媒

tetrahydrofuran

反応条件

後処理

1. 1
   温度heated
2. 2
   温度under reflux at 100° C. for 7.5 hrs
3. 3
   温度heated
4. 4
   温度under reflux for 16 hrs
5. 5
   温度After being cooled to room temperature
6. 6
   ろ過the precipitate was collected by filtration

実験手順

A 2 mol/L aqueous solution of sodium hydroxide (0.43 mL) was added to a solution of ethyl 4′-(2-[(1S,2R)-2-hydroxy-2-(4-hydroxyphenyl)-1-methylethylamino]ethoxy)biphenyl-4-carboxylate (0.15 g), ethanol (20 mL) and tetrahydrofuran (5 mL). The mixture was stirred at 60° C. for 16 hrs, and heated under reflux at 100° C. for 7.5 hrs. A 2 mol/L aqueous solution of sodium hydroxide (0.17 mL) was added, and heated under reflux for 16 hrs. After being cooled to room temperature, 2 mol/L hydrochloric acid (0.60 mL) was added, and the precipitate was collected by filtration to afford the title compound as a pale yellow amorphous (0.13 g). The structure and physical data were shown in table 3.

出典