反应详情

To a dry 18×250 mm test tube, 2-Chloro-3,6-difluorobenzaldehyde (1.00 g, 5.66 mmol) and THF (10.0 mL, 123 mmol) were added. The reaction tube was evacuated and filled with N2 3 times. Methylmagnesium bromide (0.810 g, 6.80 mmol) 1.0 M in butyl ether was added slowly at 0° C. The reaction mixture was stirred at room temperature overnight. 5 mL of sat. aq. NH4Cl was added to quench the reaction at 0° C. Diethyl ether was added and aq. layer was extracted with ether 3 times. The combined organic layers were dried over Na2SO4 and the solvent was removed in vacuo. The material was not further purified and ready for the next step.

1. additionwere added
2. customThe reaction tube was evacuated
3. additionfilled with N2 3 times
4. customto quench
5. customthe reaction at 0° C
6. extractionaq. layer was extracted with ether 3 times
7. dry with materialThe combined organic layers were dried over Na2SO4
8. customthe solvent was removed in vacuo
9. customThe material was not further purified and ready for the next step