Ethyl Acetate → HCID 68536998, compound

Temperature

0 °C

To a mixture of 3-fluoro-4-(trifluoromethyl)benzonitrile (12.1 g, 63.9 mmol) and the compound of Preparation 8 (21.0 g, 160.0 mmol) in tetrahydrofuran (345 ml), at 0° C. and under nitrogen, was added dropwise potassium tert-butoxide (1M in tetrahydrofuran, 70.3 ml, 70.3 mmol). The reaction mixture was stirred at 0° C. for 1 h and then allowed to warm to room temperature. To the mixture was added ethyl acetate (200 ml) and saturated aqueous ammonium chloride solution (250 ml) and the two layers were separated. The organic phase was washed with saturated aqueous ammonium chloride solution, water and brine, dried (MgSO4) and concentrated in vacuo. To the residue was added cyclohexane (100 ml) and the mixture was allowed to stand for 1 h. The solid residue was collected by filtration and dried to give the title compound (16.3 g).

1. temperatureto warm to room temperature
2. customthe two layers were separated
3. washThe organic phase was washed with saturated aqueous ammonium chloride solution, water and brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo
6. additionTo the residue was added cyclohexane (100 ml)
7. waitto stand for 1 h
8. filtrationThe solid residue was collected by filtration
9. customdried

ORD record

ord-4bc9b82ea0424a3f8d14797e9ec3dd50

Source dataset

uspto-grants-2009_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07608604B2