反応 #833532

反応方程式

acryloyl chloride

cyclopentadiene

acryloyl chloride

→

norbornene-5-carbonylchloride

反応条件

後処理

1. 1
   その他digital thermometer, glass stopper, an addition funnel with a nitrogen gas purge
2. 2
   workup.ADDITIONwas added drop
3. 3
   その他wise to the reaction over about three hours
4. 4
   温度while maintaining the reaction temperature between 0-10° C
5. 5
   その他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
   その他collecting 533 g of the title product
9. 9
   workup.DISTILLATIONdistilling at 54-56° C. at a pressure of 300 milliTorr

実験手順

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.

出典