2-吗啉-4-基-1-苯基乙酮

反应条件: temp:110.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 2-fluoroacetophenone (19.9 g), morpholine (21 cc) and potassium carbonate (27.6 g) in dimethyl sulphoxide (32 cc) is heated at 110° C. for 30 hours. The reaction mixture is diluted with water (100 cc) and extracted with ethyl acetate (4×100 cc); the organic solution is washed with distilled water (100 cc), dried over magnesium sulphate and concentrated to dryness under reduced pressure (2.7 kPa). The residue is chromatographed on a silica gel column (0.04-0.063 mm, diameter 9 cm, height 40 cm), eluting with a mixture of cyclohexane and ethyl acetate (80/20 by volume) and collecting 250 cc fractions. Fraction 24 to 44 are combined and concentrated to dryness under reduced pressure (2.7 kPa). 2-(4-Morpholinyl)acetophenone (4.72 g) is obtained which is used as such for the subsequent syntheses. extracted with ethyl acetate (4×100 cc) the organic solution is washed with distilled water (100 cc) dried over magnesium sulphate concentrated to dryness under reduced pressure (2.7 kPa) The residue is chromatographed on a silica gel column (0.04-0.063 mm, diameter 9 cm, height 40 cm) eluting with a mixture of cyclohexane and ethyl acetate (80/20 by volume) collecting 250 cc fractions concentrated to dryness under reduced pressure (2.7 kPa)

反应条件: temp:110.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 2-fluoroacetophenone (19.9 g), morpholine (21 cc) and potassium carbonate (27.6 g) in dimethyl sulphoxide (32 cc) is heated at 110° C. for 30 hours. The reaction mixture is diluted with water (100 cc) and extracted with ethyl acetate (4×100 cc); the organic solution is washed with distilled water (100 cc), dried over magnesium sulphate and concentrated to dryness under reduced pressure (2.7 kPa). The residue is chromatographed on a silica gel column (0.04-0.063 mm, diameter 9 cm, height 40 cm), eluting with a mixture of cyclohexane and ethyl acetate (80/20 by volume) and collecting 250 cc fractions. Fraction 24 to 44 are combined and concentrated to dryness under reduced pressure (2.7 kPa). 2-(4-Morpholinyl)acetophenone (4.72 g) is obtained which is used as such for the subsequent syntheses. extracted with ethyl acetate (4×100 cc) the organic solution is washed with distilled water (100 cc) dried over magnesium sulphate concentrated to dryness under reduced pressure (2.7 kPa) The residue is chromatographed on a silica gel column (0.04-0.063 mm, diameter 9 cm, height 40 cm) eluting with a mixture of cyclohexane and ethyl acetate (80/20 by volume) collecting 250 cc fractions concentrated to dryness under reduced pressure (2.7 kPa)

反应条件: temp:110.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 2-fluoroacetophenone (19.9 g), morpholine (21 cc) and potassium carbonate (27.6 g) in dimethyl sulphoxide (32 cc) is heated at 110° C. for 30 hours. The reaction mixture is diluted with water (100 cc) and extracted with ethyl acetate (4×100 cc); the organic solution is washed with distilled water (100 cc), dried over magnesium sulphate and concentrated to dryness under reduced pressure (2.7 kPa). The residue is chromatographed on a silica gel column (0.04-0.063 mm, diameter 9 cm, height 40 cm), eluting with a mixture of cyclohexane and ethyl acetate (80/20 by volume) and collecting 250 cc fractions. Fraction 24 to 44 are combined and concentrated to dryness under reduced pressure (2.7 kPa). 2-(4-Morpholinyl)acetophenone (4.72 g) is obtained which is used as such for the subsequent syntheses. extracted with ethyl acetate (4×100 cc) the organic solution is washed with distilled water (100 cc) dried over magnesium sulphate concentrated to dryness under reduced pressure (2.7 kPa) The residue is chromatographed on a silica gel column (0.04-0.063 mm, diameter 9 cm, height 40 cm) eluting with a mixture of cyclohexane and ethyl acetate (80/20 by volume) collecting 250 cc fractions concentrated to dryness under reduced pressure (2.7 kPa)