HRID2374751

反应详情

EQUATION

反应方程式

HRID 2374751 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of Intermediate D2 (4.57 g, 1 eq), methylamine (9.15 mL of a 2M solution in THF) and anhydrous magnesium sulphate (4.41 g, 2 eq) was stirred at room temperature for 16 h, filtered and the solid washed thoroughly with ethyl acetate. The combined filtrates were evaporated to a solid which was suspended in ethanol (90 mL) and sodium borohydride (1.01 g, 1.5 eq) added portionwise. The mixture stirred at room temperature for 3 h and the solvent removed in vacuo and the residue partitioned between dichloromethane and water. The organic layer was washed with brine, dried and evaporated to give the title compound as a white solid. 1H-NMR (CDCl3) δ 7.68 (4H, m), 7.56-7.58 (2H, m), 7.43-7.45 (2H, m), 3.83 (2H, s), 2.50 (3H, s); MS(APCI+) found (M+1)=266, C15H14F3N requires 265.

WORKUP

后处理

  1. filtrationfiltered
  2. washthe solid washed thoroughly with ethyl acetate
  3. customThe combined filtrates were evaporated to a solid which
  4. stirringThe mixture stirred at room temperature for 3 h
  5. customthe solvent removed in vacuo
  6. customthe residue partitioned between dichloromethane and water
  7. washThe organic layer was washed with brine
  8. customdried
  9. customevaporated