تفاعل #77418
ord-6008bb2fbb9e4cdab9922f9daf64bc80
معادلة التفاعل
الكواشف
لا شيء
ظروف التفاعل
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1درجة الحرارةwas heated
- 2درجة الحرارةat reflux for 4.75 h
- 3تركيزThe solution was concentrated in vacuo
- 4workup.ADDITIONthe residue was diluted with 1 N aqueous NaOH solution at 0° C.
- 5workup.ADDITIONthe pH was then adjusted to 8.5 by addition of 6 N aqueous HCl solution
- 6ترشيحThe precipitate was collected by filtration
- 7غسيلwashed several times with water
- 8تجفيفdried 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.