반응 #46164

반응 방정식

diisopropyl azodicarboxylate

hydroxyethylmorpholine

triphenyl phosphine

6-Hydroxy-1-oxo-3-phenyl-1H-indene-2-carboxylate isopropyl amide

→

6-(2-morpholine-4-yl ethoxy)-1-oxo-3-phenyl-1H-indene-2-carboxylate isopropyl amide

수율 99.0%

용매

benzene

tetrahydrofuran

반응 조건

후처리

1. 1
   기타was adjusted to 0° C.
2. 2
   세척The mixture was washed with brine
3. 3
   추출extracted with ethyl acetate
4. 4
   건조The separated organic layer was dried over anhydrous magnesium sulfate
5. 5
   농축concentrated
6. 6
   기타the resulting residue was purified by column chromatography

실험 절차

6-Hydroxy-1-oxo-3-phenyl-1H-indene-2-carboxylate isopropyl amide (7.0 g, 22.78 mmol) was dissolved in tetrahydrofuran:benzene (150 ml:50 ml). Then, hydroxyethylmorpholine (3.59 g, 27.33 mmol) and triphenyl phosphine (7.17 g, 27.33 mmol) were added thereto. When the temperature was adjusted to 0° C., diisopropyl azodicarboxylate (5.53 g, 27.33 mmol) was added dropwise to the mixture followed by stirring for 2 hours at room temperature. The mixture was washed with brine and extracted with ethyl acetate. The separated organic layer was dried over anhydrous magnesium sulfate, concentrated, and the resulting residue was purified by column chromatography to obtain 6-(2-morpholine-4-yl ethoxy)-1-oxo-3-phenyl-1H-indene-2-carboxylate isopropyl amide (9.5 g, yield 99%).

출처