반응 #613871

반응 방정식

2-[5-(2,4-Dichloro-phenyl)-2-methyl-6-(4-trifluoromethyl-phenyl)-pyridin-3-ylmethoxy]-2-methyl-propionic acid ethyl ester

LiOH

hydrochloric acid

→

2-[5-(2,4-Dichloro-phenyl)-2-methyl-6-(4-trifluoromethyl-phenyl)-pyridin-3-ylmethoxy]-2-methyl-propionic acid

용매

THF

water

반응 조건

후처리

1. 1
   농축The reaction mixture was concentrated under reduced pressure
2. 2
   추출the aqueous layer was extracted with dichloromethane
3. 3
   건조The combined organic phases were dried over MgSO4
4. 4
   기타the solvents were removed under reduced pressure
5. 5
   기타The residue was purified by preparative HPLC (
6. 6
   세척C18 reverse phase column, elution with a water/MeCN gradient with 0.1% TFA)
7. 7
   workup.ADDITIONThe fractions containing the product
8. 8
   기타were evaporated
9. 9
   기타to yield a white solid

실험 절차

To a solution of 200 mg of 2-[5-(2,4-Dichloro-phenyl)-2-methyl-6-(4-trifluoromethyl-phenyl)-pyridin-3-ylmethoxy]-2-methyl-propionic acid ethyl ester in 2 ml THF was added a solution of 18 mg of LiOH in 2 ml water at room temperature. After 16 h, the mixture was brought to pH 2 by addition of 1 M hydrochloric acid. The reaction mixture was concentrated under reduced pressure and the aqueous layer was extracted with dichloromethane. The combined organic phases were dried over MgSO4 and the solvents were removed under reduced pressure. The residue was purified by preparative HPLC (C18 reverse phase column, elution with a water/MeCN gradient with 0.1% TFA). The fractions containing the product were evaporated and lyophilized to yield a white solid. Yield: 22 mg.

출처