反应详情

温度

70 °C

2.43 g 7-Bromo-2,3,4,5-tetrahydro-1H-benzo[d]azepine are dissolved in 4.055 g of formic acid and 3.2 mL of formaldehyde solution was added. The mixture was stirred at 70° C. for 3.5 h and continued overnight at 25° C. The mixture was concentrated, diluted with water and 10 N NaOH to adjust to a basic pH. The mixture was then extracted with tertbutylmethylether (3×) and the organic phase dried (Na2SO4), filtered and concentrated to yield 2.48 g 7-bromo-3-methyl-2,3,4,5-tetrahydro-1H-benzo[d]azepine as oil.

1. waitcontinued overnight at 25° C
2. concentrationThe mixture was concentrated
3. additiondiluted with water and 10 N NaOH
4. extractionThe mixture was then extracted with tertbutylmethylether (3×)
5. dry with materialthe organic phase dried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated