反应详情

Sodium borohydride (0.367 g, 10.85 mmol) was added to a stirred solution of 2-bromo-2′,4′-difluoroacetophenone ([CAS 102429-07-2], 5.1 g, 21.7 mmol) in MeOH (152 mL) at 10° C. The mixture was stirred at RT for 1 h. Then, K2CO3 (4.499 g, 32.55 mmol) was added and the mixture was stirred at RT for 1 h. The mixture was filtered through diatomaceous earth and the filtrate was concentrated in vacuo. The residue was treated with water and extracted with CH2Cl2/THF. The organic layer was separated, dried (Na2SO4), filtered and the solvents evaporated in vacuo to yield I-19 (2.24 g, 66%) as a yellow oil.

1. stirringthe mixture was stirred at RT for 1 h
2. filtrationThe mixture was filtered through diatomaceous earth
3. concentrationthe filtrate was concentrated in vacuo
4. additionThe residue was treated with water
5. extractionextracted with CH2Cl2/THF
6. customThe organic layer was separated
7. dry with materialdried (Na2SO4)
8. filtrationfiltered
9. customthe solvents evaporated in vacuo
10. customto yield I-19 (2.24 g, 66%) as a yellow oil