反应详情

温度

60 °C

Prepared using general procedure 62: To chlorosulfonic acid (2.0 mL) at 0° C. under N2 was added (S)-3-(4-chloro-5-fluoroindolin-1-yl)-1-phenylpyrrolidin-2-one (1.92 g, 5.8 mmol) in portions. The reaction mixture was heated to 60° C. for 20 min. and, after cooling to RT, carefully poured onto ice-water. EtOAc was added, the phases were separated, and the aqueous layer was extracted with EtOAc (2×). The combined organic extracts were dried over MgSO4 and concentrated to give 4-((S)-3-(4-chloro-5-fluoroindolin-1-yl)-2-oxopyrrolidin-1-yl)benzene-1-sulfonyl chloride which was used without further purification. LC/MS (10%-99% CH3CN (0.035% TFA)/H2O (0.05% TFA)), m/z: M+1 obs=429.3; tR=2.14 min.

1. customPrepared
2. temperatureafter cooling to RT
3. additioncarefully poured onto ice-water
4. customthe phases were separated
5. extractionthe aqueous layer was extracted with EtOAc (2×)
6. dry with materialThe combined organic extracts were dried over MgSO4
7. concentrationconcentrated