A mixture of Boc2O (4.37 g, 20 mmol) in CH2Cl2 (50 mL) was added over aperiod of 3 hours to a solution of piperazine (3.44 g, 39.9 mmol) in CH2Cl2 (100 mL). The mixture was allowed to stir for 22 hours before the solvent was evaporated. Water (100 mL) was added to the residure and the insoluble product was removed by filtration. The aqueous solution was extracted with CH2Cl2 and the combined organic layers were evaporated to afford Boc-piperazine (3.08 g, 83%).
A solution of 12.5 g (55 mmol) of di-tert-butyl dicarbonate in 25 mL of CH2Cl2 was added dropwise to 100 g of N,"-dimethylethylenediamine (13) at 5 oC. The mixture was stirred at room temperature for 4 h and then evaporated. The residue was dissolved in 100 mL of ethyl acetate and washed with 100 mL of saturated aqueous Na2C03 and 100 mL of saturated aqueous NaCl. The organic layer was dried and evaporated to yield 9.3 g (90%) of the crude product.
A mixture of the ketone (10 mmol), titanium(IV) isopropoxide (6.0 mL, 20 mmol) and ammonia in ethyl alcohol (2 M, 25 mL, 50 mmol) was stirred under argon in a capped flask at ambient temperature for 6 h. Sodium borohydride (0.6 g, 15 mmol) was then added and the resulting mixture was stirred at room temperature for an additional 3 h. The reaction was then quenched by pouring into ammonium hydroxide (2 M, 25 mL), the resulting inorganic precipitate was filtered off, and washed with ethyl acetate (25 mLX2). The organic layer was separated and the remaining aqueous layer was extracted with ethyl acetate (25 mLX2). The combined organic solution was next extracted with hydrochloric acid (1 M, 30 mL) to separate the neutral materials. The acidic aqueous extracts were washed with ethyl acetate (50 mL), then treated with aqueous sodium hydroxide (2 M) to pH 10–12, and extracted with ethyl acetate (50 mLX3). The combined organic extracts were washed with brine (50 mL), dried (Na2SO4), and concentrated in vacuo to afford the corresponding primary amine.
BOC2O (1.2equiv) was dissolved in 3 mL of MeCN and placed in an ice bath, and DMAP(0.2equiv) was added. After 5min, 2-nitrobenzenamine(0.5mmol)in 2mL of MeCN was added dropwise in 1 min, and the reaction was allowed to proceed for 10 min. The mixture was concentrated and the residure was washed with diethyl ether. The solid was dissolved in MeOH and hydrogenated at the existence of Pd/C (10%) under 50 psi of H2 at room temperature for 2 hours. The reaction mixture was concentrated to give tert-butyl 2-aminophenylcarbamate.
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