تفاعل #354108

ord-6cd28b209fd748dfa4f8e2011b0ef456

المذيبات

ظروف التفاعل

درجة الحرارة
80°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe resulting homogeneous orange solution was then cooled to room temperature
  2. 2
    أخرىfreeze-dried
  3. 3
    أخرىto yield a brown solid which
  4. 4
    أخرىwas purified by HPLC (Q-Sepharose™, HPLC System III)
  5. 5
    أخرىover 60 minutes

الإجراء التجريبي

To a suspension of 200 mg (0.35 mmole) of 1-[2-(4-nitrophenyl)ethyl]-1,4,7,10-tetraazacyclododecane-4,7,10-triacetic acid, triethyl ester (prepared by the procedure of Example 19) in 15 ml of water was added 59 μl of NaOH (50% wt/wt, 3 eq). The mixture was stirred at 80° C. for 6 hours. The resulting homogeneous orange solution was then cooled to room temperature and freeze-dried to yield a brown solid which was purified by HPLC (Q-Sepharose™, HPLC System III) using a linear gradient of 0-10% aqueous HOAc over 60 minutes to yield (50%) of the hydrolyzed product 1-[2-(4-nitrophenyl)ethyl]-1,4,7,10-tetraazacyclododecane-4,7,10-triactic acid, and characterized by:

المصدر

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