2-烯丙氧基-苯基胺

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

实验步骤: The procedure of Example 1 is repeated using 1.95 g (12.5 mmol) of 1-oxyl-2,2,6,6-tetramethyl-4-hydroxypiperidine, 3.10 g (30 mmol) of tert-butyl nitrite, 2.4 g (25 mmol) of pyridine, 7.5 mg (0.012 mmol) of (S,S)-(+)-N,N-bis(3,5-di-tert-butylsalicylidene)-1,2-cyclohexanediaminocobalt(II) mmol) in 100 mL of chlorobenzene and 5.60 g (25 mmol) of 2-allyloxyaniline in 20 mL of chlorobenzene. The crude product obtained is purified by vacuum flash chromatography (25% ethyl acetate/heptane) to give 2.13 g of a viscous liquid in 59.0% yield. The crude product obtained is purified by vacuum flash chromatography (25% ethyl acetate/heptane)

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

实验步骤: The procedure of Example 1 is repeated using 1.95 g (12.5 mmol) of 1-oxyl-2,2,6,6-tetramethyl-4-hydroxypiperidine, 3.10 g (30 mmol) of tert-butyl nitrite, 7.5 mg (0.012 mmol) of (S,S)-(+)-N,N-bis(3,5-di-tert-butylsalicylidene)-1,2-cyclohexanediaminocobalt(II) mmol) in 100 mL of chlorobenzene and 5.60 g (25 mmol) of 2-allyloxyaniline in 20 mL of chlorobenzene. The crude product obtained is purified by vacuum flash chromatography (25% ethyl acetate/heptane) to give 2.22 g of a viscous liquid in 61.5% yield. The crude product obtained is purified by vacuum flash chromatography (25% ethyl acetate/heptane)

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

实验步骤: To a solution of 1.95 g (12.5 mmol) of 1-oxyl-2,2,6,6-tetramethylpiperidine, 3.1 g (30 mmol) of tert-butyl nitrite and 7.5 mg (0.012 mmol) of (S,S)-(+)-N,N-bis(3,5-di-tert-butylsalicylidene)-1,2-cyclohexanediaminocobalt(II) in 100 mL of pyridine at 65°-70° C. under a nitrogen atmosphere is added dropwise over 20 minutes a solution of 5.6 g (25 mmol) of 2-allyloxyaniline in 20 mL of pyridine. The evolution of gas is observed during the addition of the 2-allyloxyaniline. After the addition is complete, the reaction mixture is kept at 65°-70° C. for an additional forty minutes until gas evolution subsided. After cooling to ambient temperature, the reaction mixture is then concentrated. The residue obtained is purified by vacuum flash chromatography (heptane) to give 2.3 g of a viscous liquid in 63.7% yield. The structure is confirmed by 1Hnmr and elemental analyses. After the addition the reaction mixture is kept at 65°-70° C. for an additional forty minutes until gas evolution the reaction mixture is then concentrated The residue obtained is purified by vacuum flash chromatography (heptane)