反应详情

温度

-78 °C

1-Scheme 1 (1.0 g, 1.0 mmol) was suspended in THF (10 mL) and cooled to -78° C. Added n-BuLi (1.6M in Hexanes, 1.6 mmol) and allowed to react for 2 h. The mixture was warmed to -65° C.; 2-nitrobenzoyl chloride (1 mL, 7 mmol) was added, and the mixture was allowed to warm to room temperature overnight. Filtration followed by washing with methanol (3×25 mL), water (2×25 mL, methylene chloride (2×25 mL and finally with methanol (50 mL) gave the resin which was dried at 60° C. in vacuo. Recovered (1.0 g). IR 1740, 1520 cm-1.

1. customto react for 2 h
2. temperatureThe mixture was warmed to -65° C.
3. temperatureto warm to room temperature overnight
4. filtrationFiltration
5. washby washing with methanol (3×25 mL), water (2×25 mL, methylene chloride (2×25 mL
6. customfinally with methanol (50 mL) gave the resin which
7. customwas dried at 60° C. in vacuo
8. customRecovered (1.0 g)