반응 #8290

반응 방정식

hydrochloric acid

3-benzoylpropionic acid

potassium carbonate

formaldehyde

→

4-benzoyl-dihydro-furan-2-one

수율 84.1%

용매

water

반응 조건

후처리

1. 1
   온도warmed to 30° C.
2. 2
   workup.STIRRINGstirred for 3 additional days
3. 3
   온도heated at 50° C. for 30 min.
4. 4
   온도cooled to room temperature
5. 5
   추출The mixture is extracted with chloroform (4×200 mL)
6. 6
   세척the combined organic extracts washed with sodium carbonate (10% in water, 3×100 mL)
7. 7
   건조The solution is dried with anhydrous sodium sulfate
8. 8
   여과filtered
9. 9
   농축The filtrate is concentrated in vacuo

실험 절차

A mixture of 3-benzoylpropionic acid (18 g, 101 mmol), potassium carbonate (10 g, 75 mmol), water (45 mL) and formaldehyde (36% in water, 7.8 mL, 101 mmol) is stirred at room temperature for 5 days, warmed to 30° C. and stirred for 3 additional days. To this mixture is added concentrated hydrochloric acid (10 mL) to pH 5.0, heated at 50° C. for 30 min. and cooled to room temperature. The mixture is extracted with chloroform (4×200 mL) and the combined organic extracts washed with sodium carbonate (10% in water, 3×100 mL). The solution is dried with anhydrous sodium sulfate and filtered. The filtrate is concentrated in vacuo to yield 4-benzoyl-dihydro-furan-2-one (12 g) as a colorless liquid.

출처