반응 #73689

반응 방정식

methacryloyl chloride

4-hydroxybenzophenone

triethylamine

→

compound

수율 93.0%

4-benzoylphenyl methacrylate

수율 93.0%

용매

CH2Cl2

CH2Cl2

반응 조건

후처리

1. 1
   기타To a 100 mL round-bottomed flask equipped with a magnetic stirrer bar and an addition funnel
2. 2
   workup.ADDITIONwas added dropwise over 30 minutes
3. 3
   workup.WAITat room temperature for 3 hours
4. 4
   세척After this time, the organic mixture was washed with 0.1% NaOH (3×100 mL) and water (5×100 mL)
5. 5
   건조The combined organic layers were dried over MgSO4
6. 6
   농축concentrated in vacuo
7. 7
   기타to afford a crude product
8. 8
   기타The crude product was purified by column chromatography (100% CH2Cl2)

실험 절차

To a 100 mL round-bottomed flask equipped with a magnetic stirrer bar and an addition funnel was added 4-hydroxybenzophenone (1 g, 5.04 mmol) and CH2Cl2 (35 mL). The mixture was cooled to 0° C. and methacryloyl chloride (0.39 mL, 4.04 mmol) was added in one portion. After 30 minutes, triethylamine (0.7 mL, 5.04 mmol) dissolved in CH2Cl2 (10 mL) was added dropwise over 30 minutes. The reaction mixture was allowed to stir for a further 1 hour at 0° C. and then at room temperature for 3 hours. After this time, the organic mixture was washed with 0.1% NaOH (3×100 mL) and water (5×100 mL). The combined organic layers were dried over MgSO4 and then concentrated in vacuo to afford a crude product. The crude product was purified by column chromatography (100% CH2Cl2) to provide the compound as a white solid (yield=75%, 1 g).

출처