HRID1271036

反应详情

EQUATION

反应方程式

HRID 1271036 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1.5 g of 4-chloro-2-diisopropylaminomethyleneamino-5-phenylethynylpyrimidine, 20 mL of ethanol and 1.83 g of 2-(2-aminoethoxy)ethanol was refluxed for 18 hours. The tea colored solution was evaporated in vacuo and the residue partitioned between water and dichloromethane. The aqueous layer was washed twice more with dichloromethane and the combined organic extracts washed with water. The organic solution was dried over sodium sulfate, filtered and evaporated in vacuo. The yellow residue obtained was triturated with ether and filtered to give 0.49 g of a yellow solid, 2-amino-4-[2-(2-hydroxyethoxy)ethylamino]-5-phenylethynylpyrimidine. m.p. 128–129° C.

WORKUP

后处理

  1. temperaturewas refluxed for 18 hours
  2. customThe tea colored solution was evaporated in vacuo
  3. customthe residue partitioned between water and dichloromethane
  4. washThe aqueous layer was washed twice more with dichloromethane
  5. washthe combined organic extracts washed with water
  6. dry with materialThe organic solution was dried over sodium sulfate
  7. filtrationfiltered
  8. customevaporated in vacuo
  9. customThe yellow residue obtained
  10. customwas triturated with ether
  11. filtrationfiltered