HRID2291564

反应详情

EQUATION

反应方程式

HRID 2291564 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-Acetylpiperazine (6.23 g), 5-fluoro-2-nitrotoluene (7.51 g) and sodium carbonate (5.12 g) in dimethylformamide (40 ml) were stirred at 100° overnight, evaporated, and the residue partitioned between ethyl acetate and water. The organic layer was dried (sodium sulphate), evaporated, and the residue chromatographed over Merck (Trade Mark) t.l.c. grade silica, developing and eluting with 5% methanol in dichloromethane, yield 10.92 g of the title compound. A small portion was recrystallized from methanol/ethyl acetate, m.p. 133°-7°.

WORKUP

后处理

  1. customevaporated
  2. customthe residue partitioned between ethyl acetate and water
  3. dry with materialThe organic layer was dried (sodium sulphate)
  4. customevaporated
  5. customthe residue chromatographed over Merck (Trade Mark)
  6. washeluting with 5% methanol in dichloromethane, yield 10.92 g of the title compound
  7. customA small portion was recrystallized from methanol/ethyl acetate, m.p. 133°-7°