반응 #635705

반응 방정식

oxacycloheptadec-8-en-2-one

CH2I2

→

9-Oxa-bicyclo[15.1.0]octadecan-8-one

용매

Et2O

반응 조건

후처리

1. 1
   workup.ADDITIONwere added
2. 2
   온도the mixture was heated to reflux
3. 3
   기타was taken at 35° C
4. 4
   workup.WAITThe mixture was left to age overnight
5. 5
   기타Next morning, the mixture was quenched with saturated NH4Cl, aqueous layer
6. 6
   기타separated
7. 7
   세척the organic layer washed with NaHCO3
8. 8
   건조The organic layer was then dried over anhydrous MgSO4

실험 절차

To a dry 500 ml multi-neck round bottom flask fitted with an air stirrer, nitrogen inlet condenser and an addition funnel 8 g of ZnCu, 26 g of CH2I2, 100 ml of Et2O and 2 crystals of 12, were added and stirred. 12 g of oxacycloheptadec-8-en-2-one were added to the mixture and the mixture was heated to reflux. In 4 hours, first sample was taken at 35° C. The mixture was left to age overnight. Next morning, the mixture was quenched with saturated NH4Cl, aqueous layer separated and the organic layer washed with NaHCO3. The organic layer was then dried over anhydrous MgSO4. The gas chromatography test indicated that 8.1% of the starting alkene lactone converted to the cyclopropanated lactone.

출처