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温度

0 °C

To a solution of 6-bromo-N*4*-(1,3-dimethyl-1H-pyrazol-4-yl)-quinoline-3,4-diamine (Stage A.2, 3.15 g, 8.15 mmol) and TEA (1.36 ml, 9.79 mmol) in DCM (65 ml) was added under argon, after cooling with an ice-bath, a solution of trichloromethyl chloroformate (1.08 ml, 8.97 mmol in DCM (65 ml). The mixture was stirred for 25 min at 0° C. Then the RM was quenched with sat. aqueous NaHCO3 (300 ml) and 10 M aqueous NaOH (4 ml) and well stirred. The phases were separated and extracted with EtOAc (3×). The combined organic layers were washed with brine (2×), dried over Na2SO4, filtered and evaporated to dryness to give the title compound as a brownish solid (HPLC tR 2.29 min (Method A); M+H=360; M−H=358 MS-ES)

1. temperatureafter cooling with an ice-bath
2. customThen the RM was quenched with sat. aqueous NaHCO3 (300 ml) and 10 M aqueous NaOH (4 ml)
3. stirringwell stirred
4. customThe phases were separated
5. extractionextracted with EtOAc (3×)
6. washThe combined organic layers were washed with brine (2×)
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. customevaporated to dryness