반응 #1381661

반응 방정식

4-hydroxy-6-chloro-8-trifluoromethoxychroman-4-yl carboxylic acid, methyl ester

KOH H2O

→

4-Hydroxy-6-chloro-8-trifluoromethoxychroman-4-yl carboxylic acid

용매

iso-propanol

반응 조건

후처리

1. 1
   온도the mixture was refluxed overnight
2. 2
   농축The resultant solution was partially concentrated
3. 3
   추출The very turbid mixture was extracted with ether (3×)
4. 4
   건조the combined organic phase was dried (Na2SO4)
5. 5
   농축concentrated
6. 6
   기타The crude product was purified via prep-HPLC (CH3CN:0.1M ammonium acetate (30:60))
7. 7
   농축The fractions of interest were partly concentrated
8. 8
   추출extracted with ether
9. 9
   세척The combined organic layers were washed with water
10. 10
    건조dried (Na2SO4)
11. 11
    농축concentrated
12. 12
    기타yielding 0.24 g (10% over steps (vi)–(ix))

실험 절차

A solution of 4-hydroxy-6-chloro-8-trifluoromethoxychroman-4-yl carboxylic acid, methyl ester in iso-propanol (50 mL) was added to KOH/H2O (20%, 60 mL) and the mixture was refluxed overnight. The resultant solution was partially concentrated, and the remainder was acidified with H2SO4 (10%). The very turbid mixture was extracted with ether (3×), and the combined organic phase was dried (Na2SO4) and concentrated. The crude product was purified via prep-HPLC (CH3CN:0.1M ammonium acetate (30:60)). The fractions of interest were partly concentrated and extracted with ether. The combined organic layers were washed with water, dried (Na2SO4), and concentrated, yielding 0.24 g (10% over steps (vi)–(ix)).

출처