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Part B: A suspension of 4,6-diodo-2-methylpy?midme (1.83 g, 5.29 mmol) in ammonia (2 M solution in EtOH, 10 mL) was heated, in a sealed tube, at 100 C for 18 h. The reaction mixture was cooled to RT and concentrated under reduced pressure. The solid residue was washed with EtOAc and the filtrate was concentrated under reduced pressure to give 4-amino-6-diodo-2-methylpyrimidine (1.05 g, 84%) as a pale yellow solid. LCMS (m/z): 235 (M+H)+
84%
With ammonia; In ethanol; at 100℃; for 18h;
Part B: A suspension of 4,6-diodo-2-methylpyrimidine (1.83 g, 5.29 mmol) in ammonia (2 M solution in EtOH, 10 mL) was heated, in a sealed tube, at 100 C. for 18 h. The reaction mixture was cooled to RT and concentrated under reduced pressure. The solid residue was washed with EtOAc and the filtrate was concentrated under reduced pressure to give 4-amino-6-diodo-2-methylpyrimidine (1.05 g, 84%) as a pale yellow solid. LCMS (m/z): 235 (M+H)+
(6-iodo-2-methyl-pyrimidin-4-yl)-[5-(3-ethoxy-benzenesulfonyl)-thiazol-2-yl]-amine[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
66%
Part C: A mixture of 4-amino-6-diodo-2-methylpyrimidine (500 mg, 2.13 mmol) and NaH (60% dispersion in mineral oil, 170 mg, 4.25 mmol) in DMF (15 mL) was stirred at RT for 30 min. A solution of Intl-A (741 mg, 2.13 mol) in DMF (7 mL) was added, and the reaction mixture was stirred at RT for 1 h. The reaction mixture was poured into EtOAc (ca. 100 mL) and water (ca. 25 mL), IM aqueous HCl was added to give pH = 7, and the layers were separated. The organic layer was dried (Na2SO4) and concentrated under reduced pressure. The residue was purified by flash chromatography, elution with 40-75% EtOAc in hexanes, to give Int-6 (710 mg, 66%) as an off-white solid. LCMS (m/z): 503 (M+H)+
66%
Part C: A mixture of 4-amino-6-diodo-2-methylpyrimidine (500 mg, 2.13 mmol) and NaH (60% dispersion in mineral oil, 170 mg, 4.25 mmol) in DMF (15 mL) was stirred at RT for 30 min. A solution of Intl-A (741 mg, 2.13 mol) in DMF (7 mL) was added, and the reaction mixture was stirred at RT for 1 h. The reaction mixture was poured into EtOAc (ca. 100 mL) and water (ca. 25 mL), 1M aqueous HCl was added to give pH=7, and the layers were separated. The organic layer was dried (Na2SO4) and concentrated under reduced pressure. The residue was purified by flash chromatography, elution with 40-75% EtOAc in hexanes, to give Int-6 (710 mg, 66%) as an off-white solid. LCMS (m/z): 503 (M+H)+
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