تفاعل #354106

ord-6ee4a2814dec4c3ab9c1c948125c0f29

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas refluxed under a nitrogen atmosphere for 5 hours
  2. 2
    تركيزThe solution was then concentrated to dryness in vacuo
  3. 3
    أخرىto leave a solid residue
  4. 4
    أخرىThis was purified by chromatography (silica gel, Solvent System 6)

الإجراء التجريبي

A solution of α-(2-methoxy-5-nitrophenyl)-1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetic acid, tetramethyl ester (prepared by the procedure of Example 10) in concentrated HCl (5 ml, J. T. Baker ULTREX) was refluxed under a nitrogen atmosphere for 5 hours. The solution was then concentrated to dryness in vacuo to leave a solid residue. This was purified by chromatography (silica gel, Solvent System 6) to yield the title product as an off-white solid (209 mg). This material was converted to the tetrahydrochloride salt and was characterized by:

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05652361uspto-grants-1997_07