反应详情

温度

50 °C

Stir at 50° C. for 10 min. a mixture of 3-(4-pyridinylamino)-1H-indole-2-carboxylic acid (2.0 g, 8 mmol), KI (10 mg) and Cs2CO3 (2.8 g, 8.6 mmol) in DMF (125 mL). Allow to cool to ambient temperature and then cool in an ice bath. Add 2-chloro-N,N-diethylacetamide (1.077 g, 0.9 mmol) and allow to warm to ambient temperature. Add a brine solution to the reaction and extract with EtOAc (3×). Wash the extract with brine and water, dry (MgSO4), filter and concentrate under vacuum to give a semi-solid. Flash chromatograph over silica gel eluting first with EtOAc and 10% MeOH/EtOAc and obtain 0.317 g the title compound as a solid: MS 367(M+H); HPLC: Rt=4.75 min. (95/5/0.1 (A) 5/95/0.1 (B) Water/CAN/Formic Acid YMC ODS-A 2×50 mm 1 mL/min Gradient Composition: 100% A for 0.1 min Linear Gradient to 100% B at 2 min Hold until 3.5 min).

1. temperatureAllow to cool to ambient temperature
2. temperaturecool in an ice bath
3. temperatureto warm to ambient temperature
4. customto the reaction
5. extractionextract with EtOAc (3×)
6. washWash the
7. extractionextract with brine and water
8. dry with materialdry (MgSO4)
9. filtrationfilter
10. concentrationconcentrate under vacuum
11. customto give a semi-solid