تفاعل #1765238

ord-03a3886f4a034ca89ad710ad2487fe3b

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe reaction heated
  2. 2
    درجة الحرارةat reflux for 8 hours
  3. 3
    درجة الحرارةAfter cooling
  4. 4
    أخرىthe reaction was quenched with aqueous 1N hydrochloric acid
  5. 5
    غسيلwashed with ether (3×30 mL)
  6. 6
    درجة الحرارةThe pH of the aqueous phase was then raised to 10-11 with 50 wt. percent aqueous sodium hydroxide
  7. 7
    استخلاصextracted with ether (3×50 mL)
  8. 8
    تجفيفThe organics were dried (MgSO4)
  9. 9
    ترشيحfiltered
  10. 10
    أخرىsolvent removed in vacuo

الإجراء التجريبي

Sodium hydride (60 wt. percent oil dispersion, 560 mg, 14 mmol) was added to a stirred solution of 2-aminopropanol (1.2 mL, 14 mmol) in THF (25 mL). After 30 minutes, 2,6-dichloropyridine (2.0 g, 14 mmol) was added and the reaction heated at reflux for 8 hours. After cooling, the reaction was quenched with aqueous 1N hydrochloric acid and washed with ether (3×30 mL). The pH of the aqueous phase was then raised to 10-11 with 50 wt. percent aqueous sodium hydroxide and extracted with ether (3×50 mL). The organics were dried (MgSO4), filtered and solvent removed in vacuo leaving 2.2 g of a yellow oil.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08008487B2uspto-grants-2011_08