反应详情

温度

60 °C

An acetonitrile solution (250 mL) containing the intermediate from Step A (6.14 g, 40.2 mmol) and NIS (9.33 g, 41.4 mmol) was heated at 60° C. for 3 hours. The reaction solution was cooled to room temperature and concentrated to approximately 70 mL volume. The reaction was then diluted with water (ca 400 mL). The suspension was stirred for 10 minutes and then filtered. The solid was air dried on the filter to give the indicated product. The material was used in Step C without further purification. 1H NMR (400 MHz, CH 3 CN-d3): δ 1.52 (broad s, 1H); 7.62 (d, J=1.7 Hz, 1H); 7.44 (d, J=8.6 Hz, 1H); 7.21 (dd, J=8.6, 1.7 Hz, 1H). m/z=279.0 (M+H).

1. temperatureThe reaction solution was cooled to room temperature
2. concentrationconcentrated to approximately 70 mL volume
3. additionThe reaction was then diluted with water (ca 400 mL)
4. filtrationfiltered
5. customdried on the
6. filtrationfilter
7. customto give the indicated product
8. customThe material was used in Step C without further purification