반응 #160538

반응 방정식

hydrochloric acid

4-[6-(2-benzyloxycarbonylaminoethyloxy)-3-cyanoindol-1-yl]-2-methoxymethoxybenzoic acid ethyl ester

ethanol

lithium hydroxide mono hydrate

hydrochloric acid

→

title compound

수율 79.9%

4-[6-(2-Benzyloxycarbonylaminoethyloxy)-3-cyanoindol-1-yl]-2-hydroxybenzoic acid

수율 79.9%

용매

water

tetrahydrofuran

반응 조건

후처리

1. 1
   workup.STIRRINGthis mixture was stirred at 50° C. for 5 hours
2. 2
   농축this mixture was concentrated under reduced pressure until this solvent volume
3. 3
   여과The precipitated solid was collected by filtration
4. 4
   세척washed with water, methanol and ether

실험 절차

To a solution of 4-[6-(2-benzyloxycarbonylaminoethyloxy)-3-cyanoindol-1-yl]-2-methoxymethoxybenzoic acid ethyl ester (0.14 g) in a mixed solvent of ethanol (2.5 mL), tetrahydrofuran (5 mL), and water (2.5 mL) was added lithium hydroxide mono hydrate (0.03 g), and this mixture was stirred at room temperature for 3 hours. To this reaction mixture was added 2 mol/L hydrochloric acid (0.75 mL), and this mixture was stirred at 50° C. for 5 hours. This reaction mixture was treated 1 mol/L hydrochloric acid (5 mL), and this mixture was concentrated under reduced pressure until this solvent volume became one-third. The precipitated solid was collected by filtration, and washed with water, methanol and ether to give the title compound (0.097 g)

출처