反应详情

温度

50 °C

8.9 g (25 mmol) of 6-benzyloxy-4-(methylsulfonyl)amino-2,2-dimethylchroman (Example 1e) were introduced in portions at 10° C. into a suspension of 0.54 g (30 mmol) of sodium hydride (60% dispersion) in 80 ml of DMA. After stirring at 50° C. for 30 min, 2.2 ml (22 mmol) of 2-methoxyethyl bromide were added dropwise at RT. The mixture was then heated to 110° C. for 1 h, concentrated in vac., the residue was treated with water and aqueous hydrochloric acid, the resinous product was taken up with EA, the solution was dried and concentrated, and the residue was chromatographed on silica gel using toluene/EA (3:1). 2.2 g of product were crystallized from appropriate fractions using petroleum ether, m.p. 66-68° C.

1. temperatureThe mixture was then heated to 110° C. for 1 h
2. concentrationconcentrated in vac
3. addition, the residue was treated with water and aqueous hydrochloric acid
4. customthe solution was dried
5. concentrationconcentrated
6. customthe residue was chromatographed on silica gel
7. custom2.2 g of product were crystallized from appropriate fractions