반응 #63647

반응 방정식

1-(2-pyrimidinyl)-4-piperazinyl propanol

diphenylmethylbromide

sodium bicarbonate

→

title compound

수율 26.0%

2-[4-[3-(diphenylmethoxy)propyl]-1-piperazinyl]pyrimidine

수율 26.0%

용매

dimethylformamide

반응 조건

후처리

1. 1
   온도The reaction mixture was refluxed overnight
2. 2
   기타dimethylformamide was evaporated under reduced pressure
3. 3
   추출the residue was extracted with methylene chloride (400 ml.)
4. 4
   기타The methylene chloride extracts were collected
5. 5
   세척washed with water
6. 6
   기타evaporated
7. 7
   기타the remaining residue was purified by HPLC
8. 8
   기타to give 1.3 g

실험 절차

To a stirred solution of 1-(2-pyrimidinyl)-4-piperazinyl propanol 3 g. (0.013 mol) in 50 mol. of dimethylformamide was added 3.3 g. (0.013 mol) of diphenylmethylbromide and 2.9 g. (0.034 mol) of sodium bicarbonate. The reaction mixture was refluxed overnight, dimethylformamide was evaporated under reduced pressure, and the residue was extracted with methylene chloride (400 ml.). The methylene chloride extracts were collected, washed with water and evaporated, and the remaining residue was purified by HPLC to give 1.3 g. (26% yield) of the title compound. The free base which was converted to the (1:1) fumarate salt; m.p 166°-168° C.

출처