HRID2214447

反应详情

EQUATION

反应方程式

HRID 2214447 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4.68 g (30 mmol) of 2,4-dihydroxy-3-nitro-pyridine in 100 ml of dimethylformamide was combined batchwise at ambient temperature with 2.88 g (60 mmol) of a 50% suspension of sodium hydride in paraffin oil and stirred for 15 minutes. Then 8.91 ml (75 mmol) of benzylbromide were added and the mixture was stirred for 24 hours at 80° C. The solution was then carefully stirred into approx. 250 ml of water and extracted three times with 70 ml of ethyl acetate. The extracts were washed with saturated sodium chloride solution, dried and evaporated down in vacuo. The residue was triturated with diethyl ether, suction filtered and dried. The product thus obtained was further processed without any purification.

WORKUP

后处理

  1. stirringthe mixture was stirred for 24 hours at 80° C
  2. extractionextracted three times with 70 ml of ethyl acetate
  3. washThe extracts were washed with saturated sodium chloride solution
  4. customdried
  5. customevaporated down in vacuo
  6. customThe residue was triturated with diethyl ether, suction
  7. filtrationfiltered
  8. customdried
  9. customThe product thus obtained
  10. customwas further processed without any purification