反应详情

To a stirred solution of the above di-ester ((7), 7.28 g, 26 mmol) in dioxane (100 mL) was added aq. 1N NaOH (30 mL). The reaction was stirred for 6 h, acidified with aq. 1N HCl (30 mL), extracted with ethyl acetate, washed with brine, dried (MgSO4) and evaporated under reduced pressure to give the corresponding acid which was used as is in the next reaction. To a stirred solution of the above acid (6.68 g, 25 mMol) under Ar in dry CH2Cl2 (75 mL) was added pyridine (2.1 mL, 25 mMol) followed by cyanuric fluoride (1.56 mL, 17 mMol). After stirring for 2 h the reaction became a thick suspension. The reaction was then evaporated under reduced pressure, taken up in ether (150 mL) and filtered through a pad of celite to remove insoluble materials. The filtrate was washed with cold water, dried (MgSO4), filtered and evaporated under reduced pressure to give the crude acid fluoride (8) as a clear oil.

1. extractionextracted with ethyl acetate
2. washwashed with brine
3. dry with materialdried (MgSO4)
4. customevaporated under reduced pressure
5. customto give the corresponding acid which
6. customas is in the next reaction
7. stirringAfter stirring for 2 h the reaction
8. customThe reaction was then evaporated under reduced pressure
9. filtrationfiltered through a pad of celite
10. customto remove insoluble materials
11. washThe filtrate was washed with cold water
12. dry with materialdried (MgSO4)
13. filtrationfiltered
14. customevaporated under reduced pressure