HRID1271036
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas refluxed for 18 hours
- customThe tea colored solution was evaporated in vacuo
- customthe residue partitioned between water and dichloromethane
- washThe aqueous layer was washed twice more with dichloromethane
- washthe combined organic extracts washed with water
- dry with materialThe organic solution was dried over sodium sulfate
- filtrationfiltered
- customevaporated in vacuo
- customThe yellow residue obtained
- customwas triturated with ether
- filtrationfiltered