تفاعل #1583

ord-977e991e320c48a5ae6360a814f9e68c

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONpoured onto ice
  2. 2
    ترشيحThe resultant aqueous mixture is filtered
  3. 3
    أخرىto obtain a solid
  4. 4
    أخرىThe solid is dried
  5. 5
    أخرىchromatographed (silica gel/2.5% ether in methylene chloride solution)

الإجراء التجريبي

A solution of isopropyl 3-(5-amino-2-chloro-4-fluorophenyl)tetrahydro-5-methyl-2,4,6-trioxo-s-triazine-1(2H)-acetate (1.0 g, 2.6 mmol) and 3-fluorophthalic anhydride (0.51 g, 3.1 mmol) in acetic acid is refluxed for 6 hours, stirred at room temperature for several days and poured onto ice. The resultant aqueous mixture is filtered to obtain a solid. The solid is dried and chromatographed (silica gel/2.5% ether in methylene chloride solution) to give the title product as a yellow foam, mp 119°-125° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05726126uspto-grants-1998_03