تفاعل #2407

ord-f570953042144533ac7122491f64e455

معادلة التفاعل

Clc1cc(Cl)ncn1
4,6-dichloropyrimidine
OCCO
ethylene glycol
[H-].[Na+]
sodium hydride
OCCOc1cc(Cl)ncn1
2-(6-chloropyrimidin-4-yloxy)ethanol

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةcooling
  2. 2
    أخرىevaporated
  3. 3
    أخرىto remove the solvent
  4. 4
    استخلاصThe residue is extracted with ethyl acetate
  5. 5
    استخلاصthe ethyl acetate extract
  6. 6
    أخرىis dried
  7. 7
    تركيزconcentrated under reduced pressure
  8. 8
    أخرىThe residue is purified by silica gel column chromatography (solvent; chloroform/ethyl acetate=5:1~2:1)

الإجراء التجريبي

To a mixture of 4,6-dichloropyrimidine (5.0 g), ethylene glycol (100 ml) and tetrahydrofuran (100 ml)is added sodium hydride (60% dispersion-type, 1.34 g) under ice-cooling. The mixture is stirred at the same temperature for two hours, and evaporated to remove the solvent. The residue is extracted with ethyl acetate, and the ethyl acetate extract is dried, and concentrated under reduced pressure. The residue is purified by silica gel column chromatography (solvent; chloroform/ethyl acetate=5:1~2:1) to give 2-(6-chloropyrimidin-4-yloxy)ethanol (5.67 g) as an oily product.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05728706uspto-grants-1998_03