تفاعل #56546

ord-01d526c28d0343faaf6133d71910b692

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصextracted with ether
  2. 2
    تجفيفThe combined ether extracts are dried over magnesium sulfate
  3. 3
    ترشيحfiltered
  4. 4
    أخرىInto the ethereal solution is bubbled dry hydrogen chloride gas until no more oily precipitate forms
  5. 5
    أخرىThe solvent is then decanted
  6. 6
    استخلاصThe purified free base is extracted into ether
  7. 7
    تجفيفdried over magnesium sulfate
  8. 8
    أخرىWhen the solvent is evaporated

الإجراء التجريبي

A mixture of 6-cyano-6-(2,4-dichlorophenyl)decyl bromide (14.2g., 0.036 mole) imidazole (10g., 0.15 mole) and 5 ml. N,N-dimethylformamide is heated at 120° C. for 24 hours. The reaction mixture is poured into water and extracted with ether. The combined ether extracts are dried over magnesium sulfate and filtered. Into the ethereal solution is bubbled dry hydrogen chloride gas until no more oily precipitate forms. The solvent is then decanted and the oily residue is taken up in acetone and neutralized with dilute ammonium hydroxide solution. The purified free base is extracted into ether and dried over magnesium sulfate. When the solvent is evaporated, a total of 6.5 g. (47.8%) of product is obtained, which is identified by nmr.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04225723uspto-grants-1980_09