반응 #1097192

반응 방정식

6-(4-Bromo-2-methyl-phenylamino)-7-fluoro-3-pent-4-enyl-3H-benzoimidazole-5-carboxylic acid methyl ester

→

clean desired product

수율 100.0%

6-(4-Bromo-2-methyl-phenylamino)-7-fluoro-3-pent-4-enyl-3H-benzoimidazole-5-carboxylic acid

수율 100.0%

용매

THF MeOH

NaOH

반응 조건

후처리

1. 1
   workup.ADDITIONis added
2. 2
   기타the organic solvents are removed under reduced pressure
3. 3
   workup.ADDITIONthe residue diluted with water and 100 mL 1:1 THF
4. 4
   기타The layers are separated
5. 5
   추출the aqueous layer extracted with ethyl acetate
6. 6
   건조The combined organic extracts are dried (Na2SO4)
7. 7
   농축concentrated under reduced pressure

실험 절차

6-(4-Bromo-2-methyl-phenylamino)-7-fluoro-3-pent-4-enyl-3H-benzoimidazole-5-carboxylic acid methyl ester 9b is dissolved in 1:1 THF/MeOH (10 mL) and 1 N NaOH solution (2.3 mL) is added. After 5 hours, the organic solvents are removed under reduced pressure and the residue diluted with water and 100 mL 1:1 THF:ethyl acetate. The layers are separated and the aqueous layer extracted with ethyl acetate. The combined organic extracts are dried (Na2SO4) and concentrated under reduced pressure to afford 0.39 g (100%) clean desired product as a light yellow solid.

출처