反应详情

A solution of chroman-4-ylamine (Step B) (2.550 g, 17.09 mmol) in AcOH (50 mL) at RT was treated with Br2 (3.01 g, 0.96 mL, 18.8 mmol) drop-wise. The reaction was stirred at RT until HPLC analysis showed complete consumption of starting material. The mixture was diluted with H2O (100 mL) and NaOH was added until the solution became basic. The aqueous layer was extracted with EtOAc until tlc analysis of the aqueous layer showed no evidence of the title compound. The combined organics were dried over MgSO4 and concentrated in vacuo to yield the crude compound, which was purified by flash column chromatography to afford the pure title compound. MS (APCI pos) 229 (M+H).

1. customconsumption of starting material
2. additionThe mixture was diluted with H2O (100 mL) and NaOH
3. additionwas added until the solution
4. extractionThe aqueous layer was extracted with EtOAc until tlc analysis of the aqueous layer
5. dry with materialThe combined organics were dried over MgSO4
6. concentrationconcentrated in vacuo
7. customto yield the crude compound, which
8. customwas purified by flash column chromatography