تفاعل #345720

ord-85653a3932234c49b47996d6c6c4842a

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىthe reaction is then evaporated
  2. 2
    ترشيحThe suspension is filtered through a short Florisil column
  3. 3
    غسيلthe column is washed with ethyl acetate
  4. 4
    أخرىthe combined filtrates are evaporated
  5. 5
    أخرىThe residue is triturated with a minimum amount of absolute ethanol
  6. 6
    ترشيحthe title compound is filtered off
  7. 7
    أخرىdried

الإجراء التجريبي

To 3.03 g of 7-chloro-5-phenyl-1H-1,5-benzodiazepin-4-one-2-thione in a solution of 0.40 g of sodium hydroxide and 15 ml of methanol is added, with stirring a solution of 1.4 g of methyl iodide in 10 ml of methanol. Stirring is continued for 1 hour, the reaction is then evaporated and suspended in methylene chloride (30 ml). The suspension is filtered through a short Florisil column; the column is washed with ethyl acetate and the combined filtrates are evaporated. The residue is triturated with a minimum amount of absolute ethanol and the title compound is filtered off and dried.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04033947uspto-grants-1977_07