Reaktion #73689

Reaktionsgleichung

methacryloyl chloride

4-hydroxybenzophenone

triethylamine

→

compound

Ausbeute 93.0%

4-benzoylphenyl methacrylate

Ausbeute 93.0%

Lösungsmittel

CH2Cl2

CH2Cl2

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeTo 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
   WaschenAfter this time, the organic mixture was washed with 0.1% NaOH (3×100 mL) and water (5×100 mL)
5. 5
   TrocknenThe combined organic layers were dried over MgSO4
6. 6
   Einengenconcentrated in vacuo
7. 7
   Sonstigeto afford a crude product
8. 8
   SonstigeThe crude product was purified by column chromatography (100% CH2Cl2)

Vorschrift

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).

Quelle