HRID2181906
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
The title compound was prepared from 2-fluoro-5-[(3-methoxyphenyl)sulfonyl]-6-methyl-5,6-dihydrophenanthridine (100 mg, 0.26 mmol), cyclohexene (528 μL, 5.2 mmol), and 1.0 M solution of boron tribromide in dichloromethane (1.6 mL) according to the procedure and in the same manner as described in Example 105, step e. The volatile components were removed in vacuo, and the crude residue was purified by preparative liquid chromatography on a Biotage® 40 Mi column of prepacked silica gel (90 g), eluting with a gradient of 5%-30% methyl tert-butyl ether in hexane, to afford the desired compound (86 mg, 89%) as a solid, m.p. 195-196° C.;
WORKUP
后处理
- customThe volatile components were removed in vacuo
- customthe crude residue was purified by preparative liquid chromatography on a Biotage® 40 Mi column of prepacked silica gel (90 g)
- washeluting with a gradient of 5%-30% methyl tert-butyl ether in hexane