反应详情

温度

120 °C

A mixture containing compound 7A (2.5 g, 11.3 mmol), tert-butyl 2-chloroacetylcarbamate (2.4 g, 12.4 mmol), sodium hydrogen phosphate (3.2 g, 22.6 mmol) and DMA (23 mL) was heated at 120° C. for two hours. The mixture was cooled to room temperature, poured into a flask containing 400 mL of water and sonicated. The solids were filtered, rinsed with water then dried under vacuum. The solids were then taken up in 600 mL ethyl acetate and filtered over short plug of silica gel. The filtrate was concentrated down to give compound 7B (1.6 g, 39%), as a dark green solid, which was used without further purification. 1H NMR (400 MHz, DMSO-d6) δ ppm 10.21 (br. s., 1 H), 8.06-8.00 (m, 1 H), 7.69 (d, J=9.9 Hz, 1 H), 7.46 (d, J=9.3 Hz, 1 H), 1.48 (s, 9 H) ESI-MS:m/z 361.1 (M+H)+.

1. temperatureThe mixture was cooled to room temperature
2. additionpoured into a flask
3. customsonicated
4. filtrationThe solids were filtered
5. washrinsed with water
6. customthen dried under vacuum
7. filtrationfiltered over short plug of silica gel
8. concentrationThe filtrate was concentrated down