반응 #4840

반응 방정식

ether

methyl 3-bromo-3-methyl-{4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]phenyl}propanoate

tetrahydrofuran

→

3-methyl-3-{4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]phenyl}-2-propenoic acid

반응 조건

후처리

1. 1
   기타The resulting reaction mixture
2. 2
   기타the reaction
3. 3
   기타The solvent can be removed
4. 4
   workup.DISSOLUTIONthe residual oil dissolved in ether
5. 5
   기타to obtain an ether solution which
6. 6
   추출can be extracted with 1N hydrochloride acid
7. 7
   온도The resulting sodium hydroxide solution can be heated on the steam bath
8. 8
   온도cooled
9. 9
   기타to obtain a product which
10. 10
    건조The resulting ether solution can be dried with anhydrous magnesium sulfate
11. 11
    여과filtered
12. 12
    기타evaporated

실험 절차

To a solution of methyl 3-bromo-3-methyl-{4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]phenyl}propanoate in tetrahydrofuran can be added an equivalent amount of 1,5-diazabicyclo[3.4.0]nonene-5. The resulting reaction mixture can be stirred at elevated temperature until thin layer chromatographic analysis of a reaction sample indicates the reaction to be complete. The solvent can be removed and the residual oil dissolved in ether to obtain an ether solution which can be extracted with 1N hydrochloride acid and then by 2N sodium hydroxide solution. The resulting sodium hydroxide solution can be heated on the steam bath, cooled and made acidic with concentrated hydrochloric acid to obtain a product which can be isolated from the aqueous phase with ether. The resulting ether solution can be dried with anhydrous magnesium sulfate, filtered, and evaporated to give 3-methyl-3-{4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]phenyl}-2-propenoic acid.

출처