反应详情

Crude iodide 2 was taken up in deionized (DI) water, which separated the product from small amounts of a dark, insoluble residue. The water solution was decanted to a second flask and a solution of ammonium hexafluorophosphate (950 mg, ca. 5.8 mmol) in 10 mL of DI water was added in portions. An oil separated during the addition, and the supernatant solution was decanted out. The oil was crushed in cold (0° C.), and subsequently recrystallized in methanol. Yield: 1.3 g (73% from 1). 1H-NMR (δ, CDCl3): 8.67 (s, 1H, N—CH—N); 7.39 (m, 3H, C6H5); 7.29 (d, 2H, C6H5); 5.24 (s, 2H, NCH2); 4.21 (s, 3H, OCH3); 2.27 (s, 3H, CH3); 2.17 (s, 3H, CH3).

1. customseparated the product from small amounts of a dark, insoluble residue
2. customThe water solution was decanted to a second flask
3. customAn oil separated during the addition
4. customthe supernatant solution was decanted out
5. customThe oil was crushed in cold (0° C.)
6. customsubsequently recrystallized in methanol