反应详情

温度

80 °C

To DMF (1.74 gm, 0.023 moles) cooled to 0° C. under nitrogen atmosphere, Phosphorous oxy chloride (3.5 gm, 0.022 moles) was added in portions and stireed for 15 mins. To this was added a solution of the product of step 1 (2.5 gm, 0.011 mole) in dichloro ethane (18 ml) at 0° C. and heated to 80° C. for 2 hrs. The solvents were evaporated under reduced pressure. The residue was dissolved in water, basified with NaOH and extracted with ethyl acetate. The ethyl acetate extract was washed with water & brine, dried over sodium sulphate and evaporated under reduced pressure. The crude product was purified by column chromatography (eluent: 40% EtOAC in hexane) to yield 900 mg (31%) of product as solid.

1. customThe solvents were evaporated under reduced pressure
2. dissolutionThe residue was dissolved in water
3. extractionextracted with ethyl acetate
4. extractionThe ethyl acetate extract
5. washwas washed with water & brine
6. dry with materialdried over sodium sulphate
7. customevaporated under reduced pressure
8. customThe crude product was purified by column chromatography (eluent: 40% EtOAC in hexane)