HRID2181903

反应详情

EQUATION

反应方程式

HRID 2181903 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The title compound was prepared from 2-fluoro-5-[(4-methoxyphenyl)sulfonyl]-6-methyl-5,6-dihydrophenanthridine (220 mg, 0.57 mmol), cyclohexene (1.2 mL, 11.5 mmol), and 1.0 M solution of boron tribromide in dichloromethane (3.4 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 product (164 mg, 77%) as a solid, m.p. 216-218° C.;

WORKUP

后处理

  1. customThe volatile components were removed in vacuo
  2. customthe crude residue was purified by preparative liquid chromatography on a Biotage® 40 Mi column of prepacked silica gel (90 g)
  3. washeluting with a gradient of 5%-30% methyl tert-butyl ether in hexane