تفاعل #324183

ord-09acd5ebf5c742e09a29a5976bd57e20

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصthe solution extracted with chloroform
  2. 2
    أخرىThe extract was dried
  3. 3
    تركيزconcentrated
  4. 4
    أخرىIt was chromatographed on silica gel (Silicar CC-4)
  5. 5
    أخرىto give 5.5 g of a cut which
  6. 6
    أخرىwas obtained

الإجراء التجريبي

A solution of 6.9 g of 4-(4-chlorophenyl)-5-(2-thienyl)-1H-2-imidazolethiol in 40 ml of dimethylformamide and 1.5 ml of diisopropylamine was pressured in a bomb with 3 g of tetrafluoroethylene and shaken until there was no further pressure drop. The bomb contents were poured into water, the pH adjusted to 8 and the solution extracted with chloroform. The extract was dried and concentrated. It was chromatographed on silica gel (Silicar CC-4) to give 5.5 g of a cut which was dissolved in hot 1-chlorobutane. On cooling 4.5 g of product was obtained, m.p. 161.5°-163° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04159338uspto-grants-1979_06