HRID1158549

反应详情

EQUATION

反应方程式

HRID 1158549 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a 250 mL round-bottomed flask fitted with a reflux condenser was added 11,12-bis(8-isocyanatooctyl)docosane (diamer diisocyanate, Cognis Corp.) (11.74 g, 19.03 mmol) and 2-amino-6-methylpyrimidin-4(1H)-one (5 g, 40.0 mmol) in Pyridine (50 mL) to give a white suspension. The mixture was heated to 95 deg/C. under argon and stirred for 24 h. The pyridine was removed and the residue was taken up in chloroform. The hazy solution was filtered and the resulting clear solution was concentrated to about 100 ml and the viscous solution was poured into a rapidly stirring solution (1.5 L) of MeOH upon which a white solid formed. The white powder was collected by vacuum filtration and dried at 50 deg for 24 h to give 1,1′-(9,10-didecyloctadecane-1,18-diyl)bis(3-(6-methyl-4-oxo-1,4-dihydropyrimidin-2-yl)urea) (14.8 g)

WORKUP

后处理

  1. customIn a 250 mL round-bottomed flask fitted with a reflux condenser
  2. customto give a white suspension
  3. temperatureThe mixture was heated to 95 deg/C
  4. customThe pyridine was removed
  5. filtrationThe hazy solution was filtered
  6. concentrationthe resulting clear solution was concentrated to about 100 ml
  7. additionthe viscous solution was poured into a rapidly stirring solution (1.5 L) of MeOH upon which a white solid
  8. customformed
  9. filtrationThe white powder was collected by vacuum filtration
  10. customdried at 50 deg for 24 h