반응 #1596973

반응 방정식

p-hydroxybenzoic acid

8-bromo-1-octene

potassium carbonate

N,N-dimethylacetamide

→

4-(7-octenyloxy)-benzoic acid

용매

water

반응 조건

후처리

1. 1
   온도After cooled
2. 2
   추출extracted with ethyl acetate (500 mL)
3. 3
   세척washed two times with water (100 mL)
4. 4
   건조This was dried with anhydrous magnesium sulfate
5. 5
   여과filtered
6. 6
   기타The solvent was removed through concentration under reduced pressure
7. 7
   workup.DISSOLUTIONthe residue was dissolved in methanol (100 mL)
8. 8
   workup.ADDITIONgradually added
9. 9
   온도heated
10. 10
    온도under reflux for 2 hours
11. 11
    온도After cooled
12. 12
    여과the formed crystal was collected through filtration
13. 13
    세척washed with water
14. 14
    기타This was dried
15. 15
    기타to give TP-5C (63.3 g, 85%)

실험 절차

p-hydroxybenzoic acid (33.2 g), 8-bromo-1-octene (57.3 g), potassium carbonate (41.5 g) and N,N-dimethylacetamide (200 mL) were put into a 500-mL three-neck flask, and stirred at 120° C. for 5 hours. After cooled, the reaction mixture was poured into water (200 mL), extracted with ethyl acetate (500 mL), and washed two times with water (100 mL). This was dried with anhydrous magnesium sulfate and then filtered. The solvent was removed through concentration under reduced pressure, the residue was dissolved in methanol (100 mL), and a methanol solution (20 mL) of potassium hydroxide (16.8 g) was dropwise and gradually added thereto, and heated under reflux for 2 hours. After cooled, the formed crystal was collected through filtration and washed with water. This was dried to give TP-5C (63.3 g, 85%).

출처