Dimethylformamide → 3-Chloro-4,4,4-trifluoro-2-phenyl-but-2-enal

At 0° C., DMF (4.3 mL) is carefully treated with phosphoroxychloride (2.8 mL) and the mixture is stirred at rt for 20 min before 1,1,1-trifluoro-3-phenyl-propan-2-one (1.55 mL, 10 mmol) is slowly added. The reaction mixture is stirred for 2 h at 45° C. and 18 h at rt, diluted with sat. aq. Na-acetate solution (20 mL) and water (40 mL) and extracted with diethyl ether. The organic phase is separated, washed with sat. aq. NaHCO3-solution, dried over Na2SO4 and evaporated to give 3-chloro-4,4,4-trifluoro-2-phenyl-but-2-enal (2.20 g) as a pale yellow oil.

1. additionis slowly added
2. extractionextracted with diethyl ether
3. customThe organic phase is separated
4. washwashed with sat. aq. NaHCO3-solution
5. dry with materialdried over Na2SO4
6. customevaporated

ORD-Eintrag

ord-d4493b7e88f2447ab65b7d7c1a38a2a3

Quelldatensatz

uspto-grants-2011_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07951794B2