4,4,4-trifluorobutanamide

Conditions: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A mixture of 4,4,4-trifluorobutanamide (17.9 g), 2,4-bis(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane 2,4-disulfide (51.3 g) and toluene (400 mL) was stirred at 80° C. for 3 hr. The reaction mixture was purified by aminopropylsilane-bonded silica gel column chromatography (ethyl acetate), and again purified by aminopropylsilane-bonded silica gel column chromatography (ethyl acetate/hexane) to give the title compound (14.6 g) as a solid. The reaction mixture was purified by aminopropylsilane- again purified by aminopropylsilane-

Conditions: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A mixture of 4,4,4-trifluorobutanamide (17.9 g), 2,4-bis(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane 2,4-disulfide (51.3 g) and toluene (400 mL) was stirred at 80° C. for 3 hr. The reaction mixture was purified by aminopropylsilane-bonded silica gel column chromatography (ethyl acetate), and again purified by aminopropylsilane-bonded silica gel column chromatography (ethyl acetate/hexane) to give the title compound (14.6 g) as a solid. The reaction mixture was purified by aminopropylsilane- again purified by aminopropylsilane-

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a solution of 4,4,4-trifluorobutanoic acid (19.9 g) in THF (200 mL) were added oxalyl chloride (30.5 mL) and DMF (0.54 mL) at 0° C., and the mixture was stirred for 4 hr. The obtained reaction mixture was added to 28% aqueous ammonia (150 mL) at 0° C., and the mixture was stirred for 1 hr. The reaction mixture was filtration, and the filtrate was extracted with ethyl acetate. The extract was washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The obtained solid was suspended in diisopropyl ether. The precipitate was collected by filtration, washed with diisopropyl ether, and dried to give the title compound (17.9 g) as a solid. The obtained reaction mixture the mixture was stirred for 1 hr filtration the filtrate was extracted with ethyl acetate The extract was washed with saturated brine dried over magnesium sulfate concentrated under reduced pressure The precipitate was collected by filtration washed with diisopropyl ether dried

Conditions: temp:80.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A mixture of 4,4,4-trifluorobutanamide (17.9 g), 2,4-bis(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane 2,4-disulfide (51.3 g) and toluene (400 mL) was stirred at 80° C. for 3 hr. The reaction mixture was purified by aminopropylsilane-bonded silica gel column chromatography (ethyl acetate), and again purified by aminopropylsilane-bonded silica gel column chromatography (ethyl acetate/hexane) to give the title compound (14.6 g) as a solid. The reaction mixture was purified by aminopropylsilane- again purified by aminopropylsilane-

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: To a solution of 4,4,4-trifluorobutanoic acid (19.9 g) in THF (200 mL) were added oxalyl chloride (30.5 mL) and DMF (0.54 mL) at 0° C., and the mixture was stirred for 4 hr. The obtained reaction mixture was added to 28% aqueous ammonia (150 mL) at 0° C., and the mixture was stirred for 1 hr. The reaction mixture was filtration, and the filtrate was extracted with ethyl acetate. The extract was washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The obtained solid was suspended in diisopropyl ether. The precipitate was collected by filtration, washed with diisopropyl ether, and dried to give the title compound (17.9 g) as a solid. The obtained reaction mixture the mixture was stirred for 1 hr filtration the filtrate was extracted with ethyl acetate The extract was washed with saturated brine dried over magnesium sulfate concentrated under reduced pressure The precipitate was collected by filtration washed with diisopropyl ether dried