تفاعل #325049

ord-29c29a6fc91e4085ac269d14df1803ac

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    تركيزconcentrated in vacuo
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in methylene chloride
  3. 3
    غسيلwashed with water
  4. 4
    تجفيفThe methylene chloride layer was dried over 4 A molecular sieves
  5. 5
    ترشيحfiltered
  6. 6
    تركيزconcentrated in vacuo

الإجراء التجريبي

Methanol (250 ml) and sodium hydrogen cyanamide (1.92 g, 30 mmol) were added to a flask containing 2-(4-cyclohexyl-phenoxymethyl)-2-methyl-oxirane (6.15 g, 25 mmol). The reaction mixture was stirred overnight at room temperature and then concentrated in vacuo. The residue was dissolved in methylene chloride and washed with water, then saturated potassium carbonate. The methylene chloride layer was dried over 4 A molecular sieves, filtered and concentrated in vacuo to yield 5.46 g of a white solid. The white solid was recrystallized from ether to yield 1.11 g of the title compound as white crystals. A second crop yielded 0.64 g of white crystals.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08642603B2uspto-grants-2014_02