تفاعل #77418

ord-6008bb2fbb9e4cdab9922f9daf64bc80

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated
  2. 2
    درجة الحرارةat reflux for 4.75 h
  3. 3
    تركيزThe solution was concentrated in vacuo
  4. 4
    workup.ADDITIONthe residue was diluted with 1 N aqueous NaOH solution at 0° C.
  5. 5
    workup.ADDITIONthe pH was then adjusted to 8.5 by addition of 6 N aqueous HCl solution
  6. 6
    ترشيحThe precipitate was collected by filtration
  7. 7
    غسيلwashed several times with water
  8. 8
    تجفيفdried in vacuo over P2O5

الإجراء التجريبي

A suspension of 2-bromo-6-thioureidopyridine (3 g, 12.92 mmol) and chloroacetaldehyde (3.28 mL, 25.85 mmol) in ethanol (27 mL) and water (7 mL) was heated at reflux for 4.75 h. The solution was concentrated in vacuo and the residue was diluted with 1 N aqueous NaOH solution at 0° C., stirred for 10 min, and the pH was then adjusted to 8.5 by addition of 6 N aqueous HCl solution. The precipitate was collected by filtration, washed several times with water and dried in vacuo over P2O5 to obtain the titled compound (3.17 g, 96%) as a light yellow solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06706717B2uspto-grants-2004_03