thiolan-2-ylmethanamine

反応条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 7-allyl-4-chloro-5,6-diphenyl-7H-pyrrolo[2,3-d]pyrimidine (Example 3, Step B; 200 mg, 0.58 mmol) and 140 mg of (tetrahydrothiophen-2-yl)methylamine (1.20 mmol) in N,N-dimethylformamide (3 mL) was added potassium carbonate (200 mg, 1.45 mmol). The mixture was stirred for 5 minutes at 120° C. under microwave irradiation (using powerMAX™). The reaction mixture was then cooled and diluted with EtOAc (25 mL). The mixture was extracted twice with water (10 mL) and then brine. The organic layer was dried over MgSO4, filtered and the filtrate was concentrated. The residue was purified by preparative HPLC (C8 column, water, acetonitrile, 0.1% TFA) to give the title compound. The reaction mixture was then cooled The mixture was extracted twice with water (10 mL) The organic layer was dried over MgSO4 filtered the filtrate was concentrated The residue was purified by preparative HPLC (C8 column, water, acetonitrile, 0.1% TFA)

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

実験手順: A solution of 2-[(N-tbutoxycarbonlylamino)methyl]-tetrahydrothiophene 222 (500 mg, 2.3 mmol) in DCM (25 mL) was treated with trifluoroacetic acid (10 mL). The mixture was stirred at rt for 1 h before the DCM and excess TFA were removed under reduced pressure. The oily residue was triturated with diethyl ether to afford 223 as its trifluoroacetate salt (440 mg, 1.9 mmol, 83%) as an off-white solid, which was used without further purification. were removed under reduced pressure The oily residue was triturated with diethyl ether

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

実験手順: A solution of 2-[(N-tbutoxycarbonlylamino)methyl]-tetrahydrothiophene 222 (500 mg, 2.3 mmol) in DCM (25 mL) was treated with trifluoroacetic acid (10 mL). The mixture was stirred at rt for 1 h before the DCM and excess TFA were removed under reduced pressure. The oily residue was triturated with diethyl ether to afford 223 as its trifluoroacetate salt (440 mg, 1.9 mmol, 83%) as an off-white solid, which was used without further purification. were removed under reduced pressure The oily residue was triturated with diethyl ether

反応条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 7-allyl-4-chloro-5,6-diphenyl-7H-pyrrolo[2,3-d]pyrimidine (Example 3, Step B; 200 mg, 0.58 mmol) and 140 mg of (tetrahydrothiophen-2-yl)methylamine (1.20 mmol) in N,N-dimethylformamide (3 mL) was added potassium carbonate (200 mg, 1.45 mmol). The mixture was stirred for 5 minutes at 120° C. under microwave irradiation (using powerMAX™). The reaction mixture was then cooled and diluted with EtOAc (25 mL). The mixture was extracted twice with water (10 mL) and then brine. The organic layer was dried over MgSO4, filtered and the filtrate was concentrated. The residue was purified by preparative HPLC (C8 column, water, acetonitrile, 0.1% TFA) to give the title compound. The reaction mixture was then cooled The mixture was extracted twice with water (10 mL) The organic layer was dried over MgSO4 filtered the filtrate was concentrated The residue was purified by preparative HPLC (C8 column, water, acetonitrile, 0.1% TFA)

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

実験手順: A solution of 2-[(N-tbutoxycarbonlylamino)methyl]-tetrahydrothiophene 222 (500 mg, 2.3 mmol) in DCM (25 mL) was treated with trifluoroacetic acid (10 mL). The mixture was stirred at rt for 1 h before the DCM and excess TFA were removed under reduced pressure. The oily residue was triturated with diethyl ether to afford 223 as its trifluoroacetate salt (440 mg, 1.9 mmol, 83%) as an off-white solid, which was used without further purification. were removed under reduced pressure The oily residue was triturated with diethyl ether