反应 #73689

反应方程式

methacryloyl chloride

4-hydroxybenzophenone

triethylamine

→

compound

收率 93.0%

4-benzoylphenyl methacrylate

收率 93.0%

溶剂

CH2Cl2

CH2Cl2

反应条件

后处理

1. 1
   其他To 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
   洗涤After this time, the organic mixture was washed with 0.1% NaOH (3×100 mL) and water (5×100 mL)
5. 5
   干燥The combined organic layers were dried over MgSO4
6. 6
   浓缩concentrated in vacuo
7. 7
   其他to afford a crude product
8. 8
   其他The crude product was purified by column chromatography (100% CH2Cl2)

实验过程

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).

来源