HRID1699657

反应详情

EQUATION

反应方程式

HRID 1699657 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Anhydrous potassium carbonate (3.6 g, 26.1 mmol) is added to a solution of 4-(2-fluoro-4-nitrophenyl)tetrahydro-2 H-1,2-thiazine 1,1-dioxide (1.795 g, 6.54 mmol) and allyl bromide (2.0 ml, 23.1 mmol) in dry acetonitrile (25 ml). The mixture is heated to reflux for 5 min then cooled. After filtration and evaporation the residue is chromatographed over silica gel (150 g) eluting with 0-1% methanol-chloroform. The title compound is obtained as flakes (1.70 g, 83%) mp 121°.

WORKUP

后处理

  1. temperatureThe mixture is heated
  2. temperatureto reflux for 5 min
  3. temperaturethen cooled
  4. filtrationAfter filtration and evaporation the residue
  5. customis chromatographed over silica gel (150 g)
  6. washeluting with 0-1% methanol-chloroform