HRID2352178

反应详情

EQUATION

反应方程式

HRID 2352178 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 2.73 g portion of dry 4-[[4-(3-pyridinyl)-2-pyrimidinyl]amino]phenol was dissolved in 50 ml of dry dimethylformamide. A 528 mg portion of sodium hydride (50% in oil) was added, the reaction was sealed and stirred for 45 minutes. A solution of 1.33 g of allyl bromide in 10 ml of dimethylformamide was added, the sealed mixture was stirred overnight and then evaporated at 80° C. The residue was partitioned between water and chloroform. The organic phase was separated, dried and filtered. The filtrate was evaporated and the residue crystallized from chloroform-hexane, giving 1.7 g of the desired product as yellow crystals, mp 105°-108° C.

WORKUP

后处理

  1. customthe reaction was sealed
  2. stirringthe sealed mixture was stirred overnight
  3. customevaporated at 80° C
  4. customThe residue was partitioned between water and chloroform
  5. customThe organic phase was separated
  6. customdried
  7. filtrationfiltered
  8. customThe filtrate was evaporated
  9. customthe residue crystallized from chloroform-hexane