N′-BOC-N,N-氨基邻苯二甲胺

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: DEAD (2.2 M in toluen, 1.55 mL) was added dropwise to a solution of 1,4-dioxepan-6-ol (265 mg), t-butyl (1,3-dioxoisoindolin-2-yl)carbamate (560 mg) obtained in preparation example 14-(1) and triphenylphosphine (840 mg) in THF (10 mL) under ice-cooling over 3 minutes. The reaction mixture was stirred at 0° C. for 6 minutes, and further stirred at room temperature overnight The reaction mixture was concentrated under reduced pressure. After toluene (2.5 mL) was added to the resulting residue, the precipitated solid was removed by filtration. The filtrate was purified by silica gel column chromatography (ethyl acetate/n-heptane, 20%) to give the title compound (713 mg). further stirred at room temperature overnight The reaction mixture was concentrated under reduced pressure After toluene (2.5 mL) was added to the resulting residue the precipitated solid was removed by filtration The filtrate was purified by silica gel column chromatography (ethyl acetate/n-heptane, 20%)

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: DEAD (11.5 mL) was added dropwise to a solution of (R)-(−)-3-hydroxytetrahydrofuran (CAS No. 86087-24-3) (4.84 g), t-butyl (1,3-dioxoisoindolin-2-yl)carbamate (12 g) and triphenylphosphine (18.0 g) in THF (160 mL) under ice-cooling over five minutes. The reaction mixture was stirred at 0° C. for three minutes and then at room temperature for seven hours and 40 minutes. The reaction mixture was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (ethyl acetate/n-heptane, 20%) to give the title compound (12.4 g). at room temperature for seven hours 40 minutes The reaction mixture was concentrated under reduced pressure The resulting residue was purified by silica gel column chromatography (ethyl acetate/n-heptane, 20%)

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

实验步骤: A mixture of phthalic anhydride (29.63 g, 200 mmol) and tert-butylcarbazate (26.40 g, 200 mmole) in toluene was refluxed for two hours using a Dean-Stark trap. The mixture was allowed to cool and crystallize overnight. The crystals were filtered of and washed with cold toluene. The crystals were dried in vacuum. was refluxed for two hours to cool crystallize overnight The crystals were filtered of and washed with cold toluene The crystals were dried in vacuum