N-cyclohexylformamide

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To 198 grams of cyclohexylamine (2.0 grams), 399 grams of formyldiethanolamine (3.0 mole) were added, and the mixture was placed in a stirred autoclave maintained at a temperature of 150° to 155° C. and a carbon monoxide pressure of 1260 psig. After the reaction was stopped, the contents of the autoclave were removed and distilled at 15 mm Hg. The 256 grams of overhead fraction (B.P. 155°-161° C.) was shown by proton NMR analysis to be cyclohexylformamide. This corresponds to yield of 100%. maintained at a temperature of 150° to 155° C. the contents of the autoclave were removed distilled at 15 mm Hg This corresponds to yield of 100%

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To 198 grams of cyclohexylamine (2.0 grams), 399 grams of formyldiethanolamine (3.0 mole) were added, and the mixture was placed in a stirred autoclave maintained at a temperature of 150° to 155° C. and a carbon monoxide pressure of 1260 psig. After the reaction was stopped, the contents of the autoclave were removed and distilled at 15 mm Hg. The 256 grams of overhead fraction (B.P. 155°-161° C.) was shown by proton NMR analysis to be cyclohexylformamide. This corresponds to yield of 100%. maintained at a temperature of 150° to 155° C. the contents of the autoclave were removed distilled at 15 mm Hg This corresponds to yield of 100%

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To 198 grams of cyclohexylamine (2.0 grams), 399 grams of formyldiethanolamine (3.0 mole) were added, and the mixture was placed in a stirred autoclave maintained at a temperature of 150° to 155° C. and a carbon monoxide pressure of 1260 psig. After the reaction was stopped, the contents of the autoclave were removed and distilled at 15 mm Hg. The 256 grams of overhead fraction (B.P. 155°-161° C.) was shown by proton NMR analysis to be cyclohexylformamide. This corresponds to yield of 100%. maintained at a temperature of 150° to 155° C. the contents of the autoclave were removed distilled at 15 mm Hg This corresponds to yield of 100%

反応条件: temp:-15.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of cyclohexyl isocyanate (1.25 g.; 0.01 mole) in 100 ml. anhydrous 1,4-dioxane containing two drops of anhydrous triethylamine was mixed with 0.5 gram 10% Pd-on-carbon and shaken at a pressure of 50 p.s.i. of hydrogen on a Parr low pressure hydrogenator. The uptake of hydrogen was complete in two hours. Work up, as in Example 1, gave 1.15 g. of colorless oil containing a trace of isocyanate. The product was purified by slurrying the oil with Skellysolve B, chilling at -15° C. and decanting the supernatant from the crystalline formamide. After drying under high vacuum, the weight of title product was 1.06 g. (83.5% yield). The ir, nmr and glc were identical to an authentic sample. Work up, as in Example 1, gave 1.15 g The product was purified decanting the supernatant from the crystalline formamide After drying under high vacuum

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 127.2 parts of N-cyclohexylformamide and 81 parts of phosphorous acid were reacted with 137.3 parts of phosphorus trichloride at 70°C, and maintained for 5 hours at this temperature. The reaction product was dissolved in water, treated with acetone and the precipitate separated. A 25% yield of N-cyclohexyl-1-aminomethane-1,1-diphosphonic acid, based on PCl3, was obtained. maintained for 5 hours at this temperature the precipitate separated

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To the reactor described in Example 1, there is placed 99 grams cyclohexylamine, 14 grams (0.1 mole) of sodium formanilide and 150 grams of methanol. The autoclave is closed and purged with carbon monoxide, the temperature raised to 100° C. with atmospheric steam and carbon monoxide introduced at 28 kg/cm2 for about an hour. The reaction mixture is then cooled and vented, 10 milliliters of concentrated hydrochloric acid is added and the solvent is removed by distillation. Benzene is then added and the benzene solution filtered through a bed of filter acid. Distillation gives N-cyclohexyl formamide, boiling point 118°-130° C. at 3 milliliters. The expected yield is about 79%. The autoclave is closed purged with carbon monoxide introduced at 28 kg/cm2 for about an hour The reaction mixture is then cooled 10 milliliters of concentrated hydrochloric acid is added the solvent is removed by distillation Benzene is then added the benzene solution filtered through a bed of filter acid Distillation

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To 198 grams of cyclohexylamine (2.0 grams), 399 grams of formyldiethanolamine (3.0 mole) were added, and the mixture was placed in a stirred autoclave maintained at a temperature of 150° to 155° C. and a carbon monoxide pressure of 1260 psig. After the reaction was stopped, the contents of the autoclave were removed and distilled at 15 mm Hg. The 256 grams of overhead fraction (B.P. 155°-161° C.) was shown by proton NMR analysis to be cyclohexylformamide. This corresponds to yield of 100%. maintained at a temperature of 150° to 155° C. the contents of the autoclave were removed distilled at 15 mm Hg This corresponds to yield of 100%