1-羟乙基氮丙啶

反应条件: temp:10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: N-(β-hydroxyethyl)-2-aminoethanesulfonic acid, ##STR7## was prepared as follows: 2250 parts water was saturated with sulfur dioxide at 10° C. in a three-necked, round-bottom flask which was fitted with an electrical stirrer, thermometer, dropping funnel, and a gas inlet tube, 261 parts 1-aziridine-ethanol dissolved in 750 parts water was added via the dropping funnel while sulfur dioxide was bubbled into the flask and the temperature maintained at 10° C. After the addition was completed, the contents of the flask were concentrated to 600 parts and added to 3000 parts ethanol (F-30). The resulting solid was washed with 2000 parts ethanol, filtered, and dried to give 340 parts of the desired product. was fitted with an electrical stirrer was bubbled into the flask After the addition the contents of the flask were concentrated to 600 parts added to 3000 parts ethanol (F-30) The resulting solid was washed with 2000 parts ethanol filtered dried

反应条件: temp:10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: N-(β-hydroxyethyl)-2-aminoethanesulfonic acid, ##STR7## was prepared as follows: 2250 parts water was saturated with sulfur dioxide at 10° C. in a three-necked, round-bottom flask which was fitted with an electrical stirrer, thermometer, dropping funnel, and a gas inlet tube, 261 parts 1-aziridine-ethanol dissolved in 750 parts water was added via the dropping funnel while sulfur dioxide was bubbled into the flask and the temperature maintained at 10° C. After the addition was completed, the contents of the flask were concentrated to 600 parts and added to 3000 parts ethanol (F-30). The resulting solid was washed with 2000 parts ethanol, filtered, and dried to give 340 parts of the desired product. was fitted with an electrical stirrer was bubbled into the flask After the addition the contents of the flask were concentrated to 600 parts added to 3000 parts ethanol (F-30) The resulting solid was washed with 2000 parts ethanol filtered dried

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

实验步骤: (4-Chlorophenyl)(2,4-dichloro-3-phenylquinolin-6-yl)(1-methyl-1H-imidazol-5-yl)methanol (100 mg, 0.202 mmol, Example 65), 2-(aziridin-1-yl)ethanol (16.2 μL, 0.20 mmol), toluene (2 mL), and sodium hydride (60% dispersion in mineral oil, 20.2 mg, 0.51 mmol) were combined in a round bottom flask under an N2 atmosphere. The reaction solution was heated to reflux and refluxed overnight, cooled and stirred at room temperature an additional night before workup. Reaction contents were transferred to a separatory funnel with EtOAc dilution, and extracted with saturated, aqueous NH4Cl then saturated, aqueous NaHCO3 solutions. The organic phase was separated then dried over MgSO4, filtered and concentrated under reduced pressure. The crude product was purified by flash column chromatography (silica gel, 0-10% DCM/MeOH) to afford the title compound. MS (ESI): mass calcd. for C30H26Cl2N4O2, 544.1; m/z found, 545.1 [M+H]+; 1H NMR (600 MHz, CD3OD) δ ppm 8.05 (d, J=2.0 Hz, 1H), 7.74 (d, J=8.7 Hz, 1H), 7.61-7.57 (m, 2H), 7.40-7.35 (m, 2H), 7.35-7.31 (m, 1H), 7.28-7.23 (m, 6H), 6.18 (d, J=1.1 Hz, 1H), 4.51-4.44 (m, 2H), 3.37 (s, 3H), 2.50-2.39 (m, 2H), 1.48-1.37 (m, 2H), 0.97-0.94 (m, 2H). The reaction solution was heated to reflux refluxed overnight cooled Reaction contents extracted with saturated, aqueous NH4Cl The organic phase was separated then dried over MgSO4 filtered concentrated under reduced pressure The crude product was purified by flash column chromatography (silica gel, 0-10% DCM/MeOH)

反应条件: temp:10.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: N-(β-hydroxyethyl)-2-aminoethanesulfonic acid, ##STR7## was prepared as follows: 2250 parts water was saturated with sulfur dioxide at 10° C. in a three-necked, round-bottom flask which was fitted with an electrical stirrer, thermometer, dropping funnel, and a gas inlet tube, 261 parts 1-aziridine-ethanol dissolved in 750 parts water was added via the dropping funnel while sulfur dioxide was bubbled into the flask and the temperature maintained at 10° C. After the addition was completed, the contents of the flask were concentrated to 600 parts and added to 3000 parts ethanol (F-30). The resulting solid was washed with 2000 parts ethanol, filtered, and dried to give 340 parts of the desired product. was fitted with an electrical stirrer was bubbled into the flask After the addition the contents of the flask were concentrated to 600 parts added to 3000 parts ethanol (F-30) The resulting solid was washed with 2000 parts ethanol filtered dried