2-氯-4-氟苯肼盐酸盐

反应条件: temp:185.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a dry 15 mL ChemGlass pressure bottle under N2 was added 4-iodo-2-fluoro-3-formylpyridine (314 mg, 1.25 mmol), (2-chloro-4-fluorophenyl)hydrazine (210 mg, 1.31 mmol), and anhydrous NMP (5 mL). The reaction mixture was purged with argon, heated at 185° C. for 2 h, and then at 140° C. for 36 h. The reaction mixture was worked up according to the procedure described in Intermediate 69A and the crude product was purified by Biotage Silica gel chromatography using a 80 g Thompson Single Step™ silica cartridge with a linear gradient from 100% hexanes to 100% CH2Cl2 over 12 column volumes to give 63.5 mg (13.6%) of the title compound as a pale yellow solid, LC/MS (Condition B): ret. T=3.7 min, (M+H)+ 373.88, 375.88 and 149.3 mg (30.3%) of the hydrazone intermediate as a pale yellow solid, LC/MS (Condition B): ret. T=4.2 min, (M+H)+ 393.90, 395.90. The reaction mixture was purged with argon the crude product was purified by Biotage Silica gel chromatography