反应详情

triphenylphosphine (30.0 g, 114.3 mmol) is added, at ambient temperature, to a solution of commercial ethyl 4-chloro-3-oxobutanoate (18.81 g, 114.3 mmol) in 200 mL of anhydrous THF. The reaction medium is taken to reflux for 18 h before being concentrated under vacuum. The oil obtained is taken up in distilled water then washed with ether. The aqueous phase is then basified by a saturated aqueous solution of NaHCO3 (up to pH 8). After extraction with AcOEt, the organic phases are combined, dried over MgSO4, filtered then concentrated under vacuum. Purification is carried out by recrystallization from ether in order to produce, after filtration and drying, compound 5′-2 (14.96 g, 38.0 mmol, 34%) in the form of a slightly yellow solid.

1. temperatureto reflux for 18 h
2. concentrationbefore being concentrated under vacuum
3. customThe oil obtained
4. washthen washed with ether
5. extractionAfter extraction with AcOEt
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. concentrationthen concentrated under vacuum
9. customPurification
10. customis carried out by recrystallization from ether in order
11. customto produce
12. filtrationafter filtration
13. customdrying