反应 #833532

反应方程式

acryloyl chloride

cyclopentadiene

acryloyl chloride

→

norbornene-5-carbonylchloride

反应条件

后处理

1. 1
   其他digital thermometer, glass stopper, an addition funnel with a nitrogen gas purge
2. 2
   workup.ADDITIONwas added drop
3. 3
   其他wise to the reaction over about three hours
4. 4
   温度while maintaining the reaction temperature between 0-10° C
5. 5
   其他the cooling bath was removed
6. 6
   温度to warm to room temperature overnight
7. 7
   workup.DISTILLATIONThe reaction mixture was distilled under vacuum
8. 8
   其他collecting 533 g of the title product
9. 9
   workup.DISTILLATIONdistilling at 54-56° C. at a pressure of 300 milliTorr

实验过程

A 1-L, three-neck round-bottom flask equipped with a magnetic stirrer, digital thermometer, glass stopper, an addition funnel with a nitrogen gas purge, and a dry-ice cooling bath was charged with freshly distilled cyclopentadiene (248 g, 3.75 mol), which was cooled to 0° C. The addition funnel was charged with freshly distilled acryloyl chloride (317 g, 3.5 mol), which was added drop wise to the reaction over about three hours while maintaining the reaction temperature between 0-10° C. After the acryloyl chloride addition was complete, the cooling bath was removed and the reaction allowed to warm to room temperature overnight. The reaction mixture was distilled under vacuum, collecting 533 g of the title product distilling at 54-56° C. at a pressure of 300 milliTorr.

来源