HRID1030496

反应详情

EQUATION

反应方程式

HRID 1030496 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A flask containing a mixture of 2,2-diphenylethylamine (5.92 g; 3.00×10-2 mole) and 2-methylthio-1,4,5,6-tetrahydropyrimidine hydroiodide (7.74 g, 3.00×10-2 mole) was immersed in an oil bath which had been preheated to ca. 155° C. The reaction was stirred at between 150°-168° C. for 1.5 hours. The resulting yellow glass was dissolved in methanol. The methanol was evaporated and the resulting yellow oil was dissolved in dichloromethane. This solution was transferred to a separatory funnel where it was washed with 2N aqueous NaOH and saturated aqueous NaCl. After drying over anhydrous Na2SO4, the dichloromethane was evaporated giving a foam which was dissolved in methanol (125 ml). This solution was cooled to 0° C. at which time it was treated with a methanolic solution of HCl. After 10-15 minutes most of the methanol was evaporated and 2-butanone was added. After several days the crystals were collected by filtration. Recrystallization from isopropanol afforded 2-(2,2-diphenylethylamino)-1,4,5,6-tetrahydropyrimidine hydrochloride as off-white crystals: 3.80 g (40%), m.p. 180°-182° C.

WORKUP

后处理

  1. additionA flask containing
  2. customwas immersed in an oil bath
  3. customhad been preheated to ca. 155° C
  4. customThe methanol was evaporated
  5. dissolutionthe resulting yellow oil was dissolved in dichloromethane
  6. customThis solution was transferred to a separatory funnel
  7. washwhere it was washed with 2N aqueous NaOH and saturated aqueous NaCl
  8. dry with materialAfter drying over anhydrous Na2SO4
  9. customthe dichloromethane was evaporated
  10. customgiving a foam which
  11. customAfter 10-15 minutes most of the methanol was evaporated
  12. addition2-butanone was added
  13. filtrationAfter several days the crystals were collected by filtration
  14. customRecrystallization from isopropanol