反应详情

A stirred solution of 2.0 g (14.48 mmol) of 2-fluoroacetophenone (32-1) in 10 mL of ethylene glycol under nitrogen was treated with 473 uL (15.06 mmol) of hydrazine. This solution was stirred for 2 hours at room temperature and then heated at 165° C. for 40 hours. The solution was cooled to room temperature, poured into CH2Cl2 (25 mL), and extracted with H2O (2×50 mL). The organic portions were combined, dried (MgSO4), filtered and conc. in vacuo. Purification of the crude material by recrystallization from hexanes/CHCl3 gave the desired product 32-2 as a tan solid. 1H NMR (DMSO-d6): δ 7.70 (d, 1H), 7.42 (m, 2H), 7.17 (dd, 1H), 2.60 (s, 3H).

1. temperatureheated at 165° C. for 40 hours
2. temperatureThe solution was cooled to room temperature
3. extractionextracted with H2O (2×50 mL)
4. dry with materialdried (MgSO4)
5. filtrationfiltered and conc. in vacuo
6. customPurification of the crude material
7. customby recrystallization from hexanes/CHCl3