HRID1665508

反应详情

EQUATION

反应方程式

HRID 1665508 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

In a three necked flask under nitrogen equipped was dissolved 2,4-dichloro-6-morpholin-4-yl-[1,3,5]triazine (610 mg, 2.6 mmol), tributyldihydropyranylstannane (1.45 g, 3.89 mmol, 1.5 eq), and (Ph3P)2PdCl2 (150 mg, 0.21 mmol, 0.1 eq) in anhydrous dioxan (5 ml). The reaction mixture was heated under stirring to 90° C. for 16 hrs. For purification silica gel (10 g) was added to the mixture and the solvent was removed to let the product adsorbed on the silica gel. The silica gel plug was placed on a column and the mixture was flash chromatographed with hexane:ethyl acetate (10:1) to give after removal solvent the product as off white solid (345 mg=47% yield); MS (ESI) m/z 281.

WORKUP

后处理

  1. customIn a three necked flask under nitrogen equipped
  2. temperatureThe reaction mixture was heated
  3. customFor purification silica gel (10 g)
  4. additionwas added to the mixture
  5. customthe solvent was removed
  6. customchromatographed with hexane:ethyl acetate (10:1)
  7. customto give
  8. customafter removal solvent the product as off white solid (345 mg=47% yield)