반응 #47809

반응 방정식

Diisopropyl azodicarboxylate

2-hydroxyethylmorpholine

triphenylphosphine

6-Hydroxy-1-oxo-3-phenyl-1H-indene-2-carboxylic acid ethyl ester

→

titled compound

6-(2-morpholine-4-ylethoxy)-1-oxo-3-phenyl-1H-indene-2-carboxylic Acid Ethyl Ester

용매

THF benzene

반응 조건

후처리

1. 1
   workup.ADDITIONwere added
2. 2
   기타kept at 0° C
3. 3
   세척The resulting mixture washed with saturated saline
4. 4
   추출extracted with ethyl acetate
5. 5
   기타The organic layer was separated
6. 6
   건조dried over anhydrous MgSO4
7. 7
   농축concentrated under a reduced pressure
8. 8
   기타The resulting residue was purified by flash chromatography

실험 절차

6-Hydroxy-1-oxo-3-phenyl-1H-indene-2-carboxylic acid ethyl ester (2 g, 6.79 mmol) prepared in Preparation Example 2 was dissolved in THF/benzene (270 mL/90 mL) solution, and 2-hydroxyethylmorpholine (5.83 g, 44.45 mmol) and triphenylphosphine (11.66 g, 44.45 mmol) were added thereto and kept at 0° C. Diisopropyl azodicarboxylate (8.99 g, 44.45 mmol) was added dropwise to the mixture, followed by stirring for 2 hrs at room temperature. The resulting mixture washed with saturated saline and extracted with ethyl acetate. The organic layer was separated, dried over anhydrous MgSO4, and concentrated under a reduced pressure. The resulting residue was purified by flash chromatography to obtain 14 g of the titled compound (yield: 93%) as a red solid.

출처