تفاعل #451803

ord-c3ca85b0010e449b8758d7dfd7ba1914

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe mixture was heated to 100° until dissipation of the red color
  2. 2
    ترشيحThe mixture is filtered
  3. 3
    درجة الحرارةcooled
  4. 4
    استخلاصextracted with ether
  5. 5
    استخلاصThe dried extract (MgSO4)
  6. 6
    تركيزwas concentrated in vacuo

الإجراء التجريبي

This example serves to illustrate procedure B of Scheme 2. To an ice-cooled solution of 1-(2-pyrimidinyl)piperazine (16.4 g, 0.1 mole) in 1N HCl (100 mL) was added dropwise bromine (15.98 g, 0.1 mole). After stirring at 0° for 0.5 hr, the mixture was heated to 100° until dissipation of the red color had occurred. The mixture is filtered, cooled, made alkaline with 50% NaOH and extracted with ether. The dried extract (MgSO4) was concentrated in vacuo to provide 14.5 g (62%) of product, m.p. 73°-75°.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04605655uspto-grants-1986_08