تفاعل #163298

ord-66d08c1482514ff997c4bd7988b314be

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    غسيلwashed with diethyl ether (3×150 ml)
  2. 2
    استخلاصextracted with diethyl ether (3×300 ml)
  3. 3
    تركيزThe combined organic phases were concentrated under reduced pressure
  4. 4
    أخرىthe crude residue obtained
  5. 5
    أخرىwas purified by crystallization from a 1/1 hexane/ethyl acetate mixture

الإجراء التجريبي

To a solution of 2-(1H-indazol-3-ylmethoxy)-2-methylpropanoic acid (6 g; 0.026 mol) in acetone (50 ml) stirred at room temperature was added K2CO3 (6.8 g; 0.049 mol) and then, slowly, a solution of benzoyl chloride (5 ml; 0.043 mol) in acetone (30 ml). The mixture was stirred at room temperature for 24 hours and then poured into water (1 L). The solution was then brought to basic pH with 5N NaOH and washed with diethyl ether (3×150 ml). The alkaline phase was then acidified with concentrated HCl and extracted with diethyl ether (3×300 ml). The combined organic phases were concentrated under reduced pressure and the crude residue obtained was purified by crystallization from a 1/1 hexane/ethyl acetate mixture. 2 g of 2-[(1-benzoyl-1H-indazol-3-yl)methoxy]-2-methylpropanoic acid were obtained, m.p.=132-135° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08835481B2uspto-grants-2014_09