반응 #1571696

반응 방정식

6-[4-methyl-3-(trifluoromethoxy)phenoxy]pyridin-3-amine

Intermediate 31

6-[4-methyl-3-(trifluoromethoxy)phenoxy]pyridin-3-amine

acetyl chloride

→

title compound

N-{6-[4-methyl-3-(trifluoromethoxy)phenoxy]pyridin-3-yl}acetamide

용매

DCM

DCM

반응 조건

후처리

1. 1
   workup.ADDITIONwas added drop wise
2. 2
   기타The ice bath was then removed
3. 3
   workup.ADDITIONWater was added
4. 4
   기타phases were separated
5. 5
   세척The organic phase was then washed with an aqueous 15% solution of NaHCO3
6. 6
   건조dried over Na2SO4
7. 7
   여과filtered
8. 8
   농축concentrated

실험 절차

To a solution of 6-[4-methyl-3-(trifluoromethoxy)phenoxy]pyridin-3-amine (Intermediate 31, 475 mg, 1.67 mmol) and TEA (0.28 mL) in 5 mL of dry DCM under nitrogen at 0° C., acetyl chloride (0.13 mL) dissolved in 2 mL of dry DCM was added drop wise. The ice bath was then removed and the resulting solution was allowed to stir at room temperature for 30 minutes until complete conversion. Water was added and phases were separated. The organic phase was then washed with an aqueous 15% solution of NaHCO3, dried over Na2SO4, filtered and concentrated to give the title compound (502 mg) as yellow oil.

출처