HRID464651

反应详情

EQUATION

反应方程式

HRID 464651 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5 parts of 7-(3-chloropropyl)-3,7-dihydro-1,3-dimethyl-1H-purine-2,6-dione monohydrochloride, 4 parts of 3-(1,2,3,6-tetrahydro-4-pyridinyl)-1H-indole, 8 parts of sodium carbonate and 240 parts of 4-methyl-2-pentanone was stirred for 22 hours at reflux temperature. The whole was stirred till room temperature was reached. The product was filtered off and stirred in water. After filtration, the product was washed with water and stirred in water and an equivalent amount of acetic acid. The mixture was treated with ammonium hydroxide. The precipitated product was filtered off, washed with water and stirred in a mixture of acetonitrile and 2-propanol. The product was filtered off, washed with acetonitrile and dried, yielding 7 parts (98%) of 7-[3-[3,6-dihydro-4-(1H-indol-3-yl)-1(2H)-pyridinyl]propyl]-3,7-dihydro-1,3-dimethyl-1H-purine-2,6-dione; mp. 243.2° C. (compound 17).

WORKUP

后处理

  1. temperatureat reflux temperature
  2. stirringThe whole was stirred till room temperature
  3. filtrationThe product was filtered off
  4. stirringstirred in water
  5. filtrationAfter filtration
  6. washthe product was washed with water
  7. stirringstirred in water
  8. additionThe mixture was treated with ammonium hydroxide
  9. filtrationThe precipitated product was filtered off
  10. washwashed with water
  11. stirringstirred in a mixture of acetonitrile and 2-propanol
  12. filtrationThe product was filtered off
  13. washwashed with acetonitrile
  14. customdried