반응 #163298
ord-66d08c1482514ff997c4bd7988b314be
반응 방정식
반응 조건
후처리
- 1세척washed with diethyl ether (3×150 ml)
- 2추출extracted with diethyl ether (3×300 ml)
- 3농축The combined organic phases were concentrated under reduced pressure
- 4기타the crude residue obtained
- 5기타was purified by crystallization from a 1/1 hexane/ethyl acetate mixture
실험 절차
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.